CN106630657A - Carbon fiber phlogopite glass ceramics multiphase material and preparation method thereof - Google Patents
Carbon fiber phlogopite glass ceramics multiphase material and preparation method thereof Download PDFInfo
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- CN106630657A CN106630657A CN201611190381.XA CN201611190381A CN106630657A CN 106630657 A CN106630657 A CN 106630657A CN 201611190381 A CN201611190381 A CN 201611190381A CN 106630657 A CN106630657 A CN 106630657A
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- carbon fiber
- powder
- phlogopite
- preparation
- weight portions
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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
Abstract
The invention discloses a preparation method of a carbon fiber phlogopite glass ceramics multiphase material. The preparation method comprises the following steps of mixing K2CO3 powder, MgO powder, SiO2 powder and Al2O3 powder with a fluxing agent, a nucleation agent and regulators according to a ratio to obtain an even mixture; fusing and heating the mixture; at the final stage of a fusion process, injecting carbon fibers into a fusion pool through nitrogen, and fully stirring to obtain an even fusion mixture; pouring the fusion mixture into a preheated mould; annealing the fusion mixture poured into the mould; carrying out nucleation and crystallization on base glass which is obtained by annealing and contains the carbon fibers to obtain the carbon fiber phlogopite glass ceramics multiphase material. The invention also provides a carbon fiber phlogopite glass ceramics multiphase material prepared with the method. The carbon fiber phlogopite glass ceramics multiphase material is prepared from the following components: K2CO3, MgO, SiO2, Al2O3, B2O3, Cr2O3, TiO2, CaO, BaO and the carbon fibers.
Description
Technical field
The present invention relates to glass ceramic composite field, more particularly to a kind of carbon fiber Phlogopite Based Glass-Ceramics complex phase material
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.Carbon fiber be it is a kind of be high intensity, the new fiber materials of high-modulus of the phosphorus content more than 95%.Carbon is fine
Dimension density is less than metallic aluminium, but mechanical strength is higher than iron and steel, and with corrosion-resistant, high-modulus characteristic.Carbon fiber can be with
The toughening material for making devitrified glass is compound with devitrified glass to strengthen its toughness.
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 carbon fiber is combined with devitrified glass using fusion method, then first
Solve the problems, such as that carbon fiber is easily oxidized at high temperature；Its secondary solution carbon fiber equally distributed problem in the melt.
There is no that carbon fiber and Phlogopite Based Glass-Ceramics are combined using fusion method in current prior art is carried out
The preparation of carbon fiber 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
Carbon fiber is sprayed into bath and is sufficiently stirred for that preferable carbon fiber dispersion homo-effect can be obtained simultaneously by the phase with nitrogen stream, together
When the nitrogen that sprays into can manufacture non-oxidizing environment and prevent carbon fiber from aoxidizing at high temperature, and accelerate micro-bubble in molten bath
Floating of growing up is discharged.Inventor is also had found because the thermal coefficient of expansion of carbon fiber is basically identical with substrate glass, therefore can be avoided
Composite produces structural crack in heat treatment process because thermal stress is larger.
Worked according to the studies above, inventors herein propose carbon fiber Phlogopite Based Glass-Ceramics composite diphase material as described below and
Its preparation method.
A kind of preparation method of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material, comprises the steps of：
Step 1, by K2CO3Powder, MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent, regulator are mixed
It is combined into homogeneous mixture；
Step 2, mixture melting is heated；
Step 3, carbon fiber in the latter stage of melting process sprayed into fusion pool and be sufficiently stirred for as uniform by nitrogen
Molten mixture；
Step 4, molten mixture is poured into the mould through preheating；
Step 5, by the molten mixture being poured into mould annealing；
Step 6, the parent glass coring containing carbon fiber that annealing is obtained and crystallization.
Further, the weight portion of each component is respectively in step 1：The K of 6-10 weight portions2CO3, 14-20 weight portions
The SiO of MgO, 42-55 weight portion2, 10-16 weight portions Al2O3, the B of 3-6 weight portions2O3, be respectively 1-3 weight portions Cr2O3
And TiO2, be respectively 2-4 weight portions CaO and BaO and 9-18 weight portion carbon fiber.
Further, the powder diameter of each component is less than 200 mesh in step 1.
Further, carbon fiber is powder.
Further, flux is B2O3。
Further, Nucleating Agent is Cr2O3And TiO2。
Further, regulator is CaO and BaO, and regulator is used to adjust devitrified glass thermal coefficient of expansion.
Further, the melting heating in step 2 is carried out at a temperature of 1400-1580 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 450-650 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 preparation of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material is have effectively achieved.
Present invention also offers a kind of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material prepared by said method, it is included
Following components：K2CO3、MgO、SiO2、Al2O3、B2O3、Cr2O3、TiO2, CaO, BaO and carbon fiber.
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 carbon fiber Phlogopite Based Glass-Ceramics composite diphase material preparation method according to an embodiment of the invention
Schematic flow sheet.
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 6 weight portions2CO3Powder, the MgO powder of 18 weight portions, 50 weight portions
SiO2The Al of powder, 10 weight portions2O3The flux B of powder and 3 weight portions2O3Powder, the Nucleating Agent for being respectively 2 weight portions
Cr2O3Powder and TiO2Powder and it is total up to the regulator CaO powder and BaO powder of 6 weight portions and is mixed into homogeneous mixture.
Subsequently in step s 200, said mixture is melted into 4 hours at 1560 DEG C, to ensure the abundant melting of mixture.Connect
The melt stage latter stage in step S200, according to shown in step S300, the powder formed carbon fiber of 9 weight portions is passed through into nitrogen stream
Spray into bath and be sufficiently stirred for, carbon fiber is uniformly distributed in the mixture of melting so as to obtain containing uniform point
The molten mixture of the carbon fiber of cloth.As shown in step S400, the molten mixture cast that step S300 is obtained enters Jing 590
Among DEG C mould being fully warmed-up, and anneal 3 hours at a temperature of 590 DEG C, obtained the parent glass of carbon fiber-containing.Subsequently
In step S500, by the parent glass containing carbon fiber at a temperature of 640 DEG C coring 2 hours, then at a temperature of 870 DEG C
Crystallization obtains carbon fiber Phlogopite Based Glass-Ceramics composite for 4 hours.
Embodiment two
With reference to Fig. 1, in the step s 100, by the K of 6 weight portions2CO3Powder, the MgO powder of 14 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 2 weight portions
Cr2O3Powder and TiO2Powder and it is total up to the regulator CaO powder and BaO powder of 4 weight portions and is mixed into homogeneous mixture.
Subsequently in step s 200, said mixture is melted into 3 hours at 1480 DEG C, to ensure the abundant melting of mixture.Connect
The melt stage latter stage in step S200, according to shown in step S300, the powder formed carbon fiber of 12 weight portions is passed through into nitrogen
Stream sprays into bath and is sufficiently stirred for, and carbon fiber is uniformly distributed in the mixture of melting so as to obtain containing uniform
The molten mixture of the carbon fiber of distribution.As shown in step S400, the molten mixture cast that step S300 is obtained enters Jing
Among 580 DEG C of moulds being fully warmed-up, and anneal 3 hours at a temperature of 580 DEG C, obtained the parent glass of carbon fiber-containing.
Subsequently in step S500, by the parent glass containing carbon fiber at a temperature of 630 DEG C coring 2 hours, then in 850 DEG C of temperature
The lower crystallization of degree obtains carbon fiber Phlogopite Based Glass-Ceramics composite for 4 hours.
Embodiment three
With reference to Fig. 1, in the step s 100, by the K of 9 weight portions2CO3Powder, the MgO powder of 14 weight portions, 55 weight portions
SiO2The Al of powder, 16 weight portions2O3The flux B of powder and 3 weight portions2O3Powder, the Nucleating Agent for being respectively 1 weight portion
Cr2O3Powder and TiO2Powder and it is total up to the regulator CaO powder and BaO powder of 4 weight portions and is mixed into homogeneous mixture.
Subsequently in step s 200, said mixture is melted into 2 hours at 1410 DEG C, to ensure the abundant melting of mixture.Connect
The melt stage latter stage in step S200, according to shown in step S300, the powder formed carbon fiber of 10 weight portions is passed through into nitrogen
Stream sprays into bath and is sufficiently stirred for, and carbon fiber is uniformly distributed in the mixture of melting so as to obtain containing uniform
The molten mixture of the carbon fiber of distribution.As shown in step S400, the molten mixture cast that step S300 is obtained enters Jing
Among 460 DEG C of moulds being fully warmed-up, and anneal 4 hours at a temperature of 460 DEG C, obtained the parent glass of carbon fiber-containing.
Subsequently in step S500, by the parent glass containing carbon fiber at a temperature of 560 DEG C coring 3 hours, then in 920 DEG C of temperature
The lower crystallization of degree obtains carbon fiber Phlogopite Based Glass-Ceramics composite for 2 hours.
Example IV
With reference to Fig. 1, in the step s 100, by the K of 9 weight portions2CO3Powder, the MgO powder of 14 weight portions, 42 weight portions
SiO2The Al of powder, 16 weight portions2O3The flux B of powder and 3 weight portions2O3Powder, the Nucleating Agent for being respectively 1 weight portion
Cr2O3Powder and TiO2Powder and it is total up to the regulator CaO powder and BaO powder of 4 weight portions and is mixed into homogeneous mixture.
Subsequently in step s 200, said mixture is melted into 2 hours at 1410 DEG C, to ensure the abundant melting of mixture.Connect
The melt stage latter stage in step S200, according to shown in step S300, the powder formed carbon fiber of 10 weight portions is passed through into nitrogen
Stream sprays into bath and is sufficiently stirred for, and carbon fiber is uniformly distributed in the mixture of melting so as to obtain containing uniform
The molten mixture of the carbon fiber of distribution.As shown in step S400, the molten mixture cast that step S300 is obtained enters Jing
Among 460 DEG C of moulds being fully warmed-up, and anneal 4 hours at a temperature of 460 DEG C, obtained the parent glass of carbon fiber-containing.
Subsequently in step S500, by the parent glass containing carbon fiber at a temperature of 560 DEG C coring 3 hours, then in 920 DEG C of temperature
The lower crystallization of degree obtains carbon fiber Phlogopite Based Glass-Ceramics composite for 2 hours.
Embodiment five
With reference to Fig. 1, in the step s 100, by the K of 6 weight portions2CO3Powder, the MgO powder of 14 weight portions, 52 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 and it is total up to the regulator CaO powder and BaO powder of 4 weight portions and is mixed into homogeneous mixture.
Subsequently in step s 200, said mixture is melted into 3 hours at 1480 DEG C, to ensure the abundant melting of mixture.Connect
The melt stage latter stage in step S200, according to shown in step S300, the powder formed carbon fiber of 9 weight portions is passed through into nitrogen stream
Spray into bath and be sufficiently stirred for, carbon fiber is uniformly distributed in the mixture of melting so as to obtain containing uniform point
The molten mixture of the carbon fiber of cloth.As shown in step S400, the molten mixture cast that step S300 is obtained enters Jing 630
Among DEG C mould being fully warmed-up, and anneal 2 hours at a temperature of 630 DEG C, obtained the parent glass of carbon fiber-containing.Subsequently
In step S500, by the parent glass containing carbon fiber at a temperature of 630 DEG C coring 2 hours, then at a temperature of 710 DEG C
Crystallization obtains carbon fiber Phlogopite Based Glass-Ceramics composite for 3 hours.
Embodiment six
With reference to Fig. 1, in the step s 100, by the K of 8 weight portions2CO3Powder, the MgO powder of 14 weight portions, 42 weight portions
SiO2The Al of powder, 10 weight portions2O3The flux B of powder and 6 weight portions2O3Powder, the Nucleating Agent for being respectively 3 weight portions
Cr2O3Powder and TiO2Powder and it is total up to the regulator CaO powder and BaO powder of 4 weight portions and is mixed into homogeneous mixture.
Subsequently in step s 200, said mixture is melted into 3 hours at 1480 DEG C, to ensure the abundant melting of mixture.Connect
The melt stage latter stage in step S200, according to shown in step S300, the powder formed carbon fiber of 10 weight portions is passed through into nitrogen
Stream sprays into bath and is sufficiently stirred for, and carbon fiber is uniformly distributed in the mixture of melting so as to obtain containing uniform
The molten mixture of the carbon fiber of distribution.As shown in step S400, the molten mixture cast that step S300 is obtained enters Jing
Among 580 DEG C of moulds being fully warmed-up, and anneal 3 hours at a temperature of 580 DEG C, obtained the parent glass of carbon fiber-containing.
Subsequently in step S500, by the parent glass containing carbon fiber at a temperature of 630 DEG C coring 2 hours, then in 850 DEG C of temperature
The lower crystallization of degree obtains carbon fiber Phlogopite Based Glass-Ceramics composite for 4 hours.
Embodiment seven
With reference to Fig. 1, in the step s 100, by the K of 6 weight portions2CO3Powder, the MgO powder of 14 weight portions, 42 weight portions
SiO2The Al of powder, 16 weight portions2O3The flux B of powder and 3 weight portions2O3Powder, the Nucleating Agent for being respectively 1 weight portion
Cr2O3Powder and TiO2Powder and it is total up to the regulator CaO powder and BaO powder of 8 weight portions and is mixed into homogeneous mixture.
Subsequently in step s 200, said mixture is melted into 3 hours at 1480 DEG C, to ensure the abundant melting of mixture.Connect
The melt stage latter stage in step S200, according to shown in step S300, the powder formed carbon fiber of 9 weight portions is passed through into nitrogen stream
Spray into bath and be sufficiently stirred for, carbon fiber is uniformly distributed in the mixture of melting so as to obtain containing uniform point
The molten mixture of the carbon fiber of cloth.As shown in step S400, the molten mixture cast that step S300 is obtained enters Jing 580
Among DEG C mould being fully warmed-up, and anneal 3 hours at a temperature of 580 DEG C, obtained the parent glass of carbon fiber-containing.Subsequently
In step S500, by the parent glass containing carbon fiber at a temperature of 630 DEG C coring 2 hours, then at a temperature of 850 DEG C
Crystallization obtains carbon fiber Phlogopite Based Glass-Ceramics composite for 4 hours.
Embodiment eight
With reference to Fig. 1, in the step s 100, by the K of 7 weight portions2CO3Powder, the MgO powder of 14 weight portions, 42 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 and it is total up to the regulator CaO powder and BaO powder of 4 weight portions and is mixed into homogeneous mixture.
Subsequently in step s 200, said mixture is melted into 3 hours at 1480 DEG C, to ensure the abundant melting of mixture.Connect
The melt stage latter stage in step S200, according to shown in step S300, the powder formed carbon fiber of 18 weight portions is passed through into nitrogen
Stream sprays into bath and is sufficiently stirred for, and carbon fiber is uniformly distributed in the mixture of melting so as to obtain containing uniform
The molten mixture of the carbon fiber of distribution.As shown in step S400, the molten mixture cast that step S300 is obtained enters Jing
Among 580 DEG C of moulds being fully warmed-up, and anneal 3 hours at a temperature of 580 DEG C, obtained the parent glass of carbon fiber-containing.
Subsequently in step S500, by the parent glass containing carbon fiber at a temperature of 630 DEG C coring 2 hours, then in 850 DEG C of temperature
The lower crystallization of degree obtains carbon fiber Phlogopite Based Glass-Ceramics composite for 4 hours.
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 carbon fiber 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, Nucleating Agent, regulator are mixed into
Homogeneous mixture；
Step 2, mixture melting is heated；
Step 3, carbon fiber in the latter stage of melting process sprayed into fusion pool by nitrogen and be sufficiently stirred for as uniform melting
Mixture；
Step 4, the molten mixture is poured into the mould through preheating；
Step 5, by the molten mixture being poured into mould annealing；
Step 6, the parent glass coring containing carbon fiber that annealing is obtained and crystallization.
2. the preparation method of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is characterised in that institute
The weight portion for stating each component in step 1 is respectively：The K of 6-10 weight portions2CO3, 14-20 weight portions MgO, 42-55 weight portion
SiO2, 10-16 weight portions Al2O3, the B of 3-6 weight portions2O3, be respectively 1-3 weight portions Cr2O3And TiO2, be respectively 2-4 weight
The carbon fiber of the CaO and BaO and 9-18 weight portion of amount part.
3. the preparation method of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is characterised in that institute
Carbon fiber is stated for powder.
4. the preparation method of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is characterised in that institute
Flux is stated for B2O3。
5. the preparation method of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is characterised in that institute
Nucleating Agent is stated for Cr2O3And TiO2。
6. the preparation method of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is characterised in that institute
Regulator is stated for CaO and BaO.
7. the preparation method of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is characterised in that institute
State the heating of the melting in step 2 is carried out at a temperature of 1400-1580 DEG C.
8. the preparation method of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is characterised in that institute
It is 2-4 hours to state melting heat time in step 2.
9. the preparation method of carbon fiber Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is characterised in that institute
State the preheating of mould in step 4 is carried out at a temperature of 450-650 DEG C.
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、TiO2, CaO, BaO and carbon fiber.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH069244A (en) * | 1991-09-03 | 1994-01-18 | Agency Of Ind Science & Technol | Machinable ceramics, production thereof and method for hardening the same |
| CN101648775A (en) * | 2008-10-17 | 2010-02-17 | 韦鸿雁 | High-quality and high-efficiency composite production technology of glass basis fiber composite |
-
2016
- 2016-12-21 CN CN201611190381.XA patent/CN106630657A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH069244A (en) * | 1991-09-03 | 1994-01-18 | Agency Of Ind Science & Technol | Machinable ceramics, production thereof and method for hardening the same |
| 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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