CN106698956A - Carbon fiber-cordierite glass-ceramic composite material and preparation method thereof - Google Patents
Carbon fiber-cordierite glass-ceramic composite material and preparation method thereof Download PDFInfo
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- CN106698956A CN106698956A CN201611192282.5A CN201611192282A CN106698956A CN 106698956 A CN106698956 A CN 106698956A CN 201611192282 A CN201611192282 A CN 201611192282A CN 106698956 A CN106698956 A CN 106698956A
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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
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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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
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/20—Glass-ceramics matrix
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Abstract
The invention relates to a preparation method of a carbon fiber-cordierite glass-ceramic composite material. The preparation method comprises the following steps: uniformly mixing MgO powder, SiO2 powder, Al2O3 powder, a fluxing agent, a nucleating agent and a regulating agent in proportion to obtain a mixed raw material; melting and heating the obtained mixed raw material, spraying carbon fibers into a molten pool through gas flow at the last stage of the melting process and fully and uniformly stirring to obtain a molten raw material containing carbon fibers; pouring the obtained molten raw material containing the carbon fibers into a preheated mold and annealing to obtain base glass containing carbon fibers; nucleating and crystallizing the obtained base glass containing the carbon fibers to obtain the carbon fiber-cordierite glass-ceramic composite material. Through the preparation method provided by the invention, the efficient preparation of the carbon fiber-cordierite glass-ceramic composite material is effectively realized.
Description
Technical field
The present invention relates to glass ceramic composite field, more particularly, to a kind of carbon fiber-cordierite glass-ceramic
Composite diphase material and preparation method thereof.
Background technology
At present, prepare carbon fiber-devitrified glass composite diphase material and generally use sintering process, but there are many deficiencies, mainly
Have sintering process prepare devitrified glass volume density it is relatively low, the porosity is higher, glass-ceramic matrix combined with carbon fiber compared with
The problems such as difference.
Comparatively, fusion method prepare devitrified glass volume density is of a relatively high, the porosity is relatively low, but to using molten
Melt method carbon fiber combines with devitrified glass, then first have to solve the problems, such as that carbon fiber is easily oxidized in high-temperature fusant；
Its secondary solution carbon fiber equally distributed problem in the melt；Finally to solve parent glass thermal coefficient of expansion with carbon fiber not
Parent glass is unanimously caused easily to produce the problem of structural crack due to thermal stress during coring, crystallization and thermal treatment.
Carbon fiber is combined with cordierite glass-ceramic using fusion method in current there is no in the prior art, is prepared
The report of carbon fiber-cordierite glass-ceramic composite diphase material.
The content of the invention
Regarding to the issue above, inventor is had found carbon fiber in melt zone latter stage with nitrogen by substantial amounts of creative work
Stream sprays into bath and is sufficiently stirred for obtaining preferable carbon fiber dispersion homo-effect simultaneously, while the nitrogen for spraying into can be with
Manufacture non-oxidizing environment prevents carbon fiber from aoxidizing at high temperature, and accelerates the floating discharge of growing up of micro-bubble in molten bath.Hair
A person of good sense also found because the thermal coefficient of expansion of carbon fiber is slightly larger than parent glass, it is therefore desirable to add a certain amount of regulator to adjust
The thermal coefficient of expansion of whole parent glass, is allowed to the similar thermal expansion coefficient with carbon fiber, it is to avoid parent glass is in nucleus crystallization mistake
Due to structural crack caused by thermal stress in journey.
Worked according to the studies above, inventors herein propose carbon fiber-cordierite glass-ceramic composite diphase material as described below
Preparation method.
According to an aspect of the present invention, there is provided a kind of preparation method of carbon fiber-cordierite glass-ceramic composite diphase material,
Comprise the steps of：
1) by MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent, regulator are mixed in proportion,
Obtain mixed material；
2) by step 1) in obtain mixed material melting heating；
3) in step 2) in melting process latter stage by gas stream by carbon fiber spray into fusion pool in and be sufficiently stirred for
It is even, obtain the fused raw material containing carbon fiber；
4) by step 3) in the fused raw material containing carbon fiber that obtains be poured into by the mould that preheats and by moving back
Fire obtains the parent glass containing carbon fiber；
5) by step 4) in the parent glass coring containing carbon fiber that obtains and crystallization, obtain carbon fiber-cordierite micro-
Crystal glass composite diphase material.
According to one embodiment of present invention, above-mentioned steps 1) in the ratio of each powder be：MgO18-26 weight portions, SiO2
48-60 weight portions, Al2O310-24 weight portions.
According to one embodiment of present invention, above-mentioned steps 1) in flux be B2O3, Nucleating Agent is Cr2O3And P2O5, adjust
Whole dose is Na2O and BaO.
According to one embodiment of present invention, B2O3Ratio be 2-6 weight portions, Cr2O3And P2O5Ratio be respectively 1-3
Weight portion, Na2The ratio of O and BaO is altogether 4-8 weight portions.
According to one embodiment of present invention, above-mentioned steps 3) in the carbon fiber that adds for powdered.
According to one embodiment of present invention, the ratio of carbon fiber is 8-15 weight portions.
According to one embodiment of present invention, above-mentioned steps 2) in gas stream be nitrogen stream.
According to one embodiment of present invention, above-mentioned steps 2) in melting heating carried out at a temperature of 1480-1650 DEG C,
Step 4) in mould preheating temperature for 450-650 DEG C, annealing temperature be 4500-650 DEG C, step 5) in nucleation temperature be
550-750 DEG C, crystallization temperature be 750-980 DEG C.
According to one embodiment of present invention, above-mentioned steps 2) in the melting heat time be 3-6 hours, step 4) in
Annealing time be 4-8 hour, step 5) in nucleation time for 2-3 hours, crystallization time be 4-8 hours.
The present invention have effectively achieved the efficient system of carbon fiber-cordierite glass-ceramic composite diphase material by the above method
It is standby.
According to another aspect of the present invention, a kind of carbon fiber-cordierite using the preparation of above-mentioned preparation method is also provided micro-
Crystal glass composite diphase material.
The present invention prepare carbon fiber-cordierite glass-ceramic material have the porosity far below Sintering of Glass-Ceramics,
Carbon fiber with substrate glass is tightly combined, toughness of material is greatly improved the features such as.
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 that the flow of carbon fiber of the invention-cordierite glass-ceramic composite diphase material preparation method is illustrated
Figure.
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.
The present invention provides a kind of preparation method of carbon fiber-cordierite glass-ceramic composite diphase material.Reference picture 1, the preparation
Method is comprised the following steps：
S100 mixes in proportion
In the present invention, by MgO powder, SiO2Powder, Al2O3Powder, flux B2O3, Nucleating Agent Cr2O3With P2O5, adjust
Whole dose of Na2O is mixed in proportion with BaO, obtains preparing the primary raw material of cordierite glass-ceramic.Wherein above-mentioned each component
Ratio is MgO 18-26 weight portions, SiO248-60 weight portions, Al2O310-24 weight portions, flux B2O32-6 weight portions,
Nucleating Agent Cr2O31-3 weight portions and P2O51-3 weight portions, regulator Na2The common 4-8 weight portions of O and BaO, the particle diameter of powder is less than
200 mesh.
S200 is fully melted
In the present invention, the primary raw material for preparing cordierite glass-ceramic that will be obtained in S100 is molten at 1480-1650 DEG C
Melt heating 3-6 hours so that raw material fully to melt homogenizing, each chemical constituents analysis uniform.
S300 carbon fibers are sprayed into and stirred
In the present invention, in melt zone latter stage, the carbon fiber powder of 8-15 weight portions is sprayed into bath with nitrogen stream
And stir, wherein nitrogen stream act as：First is manufacture non-oxidizing atmosphere, protects carbon fiber powder not to be excessively oxidated；
Second is to promote carbon fiber powder in the dispersed of bath；3rd is to promote original micro-bubble in fused raw material
Grow up floating.
S400 casts and anneals
In the present invention, by containing carbon fiber fused raw material casting pass into 450-650 DEG C preheating mould in simultaneously
Annealing temperature annealing 4-8 lowered the temperature with stove again after as a child, obtained the parent glass of carbon fiber-containing.
S500 coring and crystallization
In the present invention, by the parent glass of carbon fiber-containing coring 2-3 hours at 550-750 DEG C, then it is warming up to 750-
980 DEG C crystallization 4-8 hours, and then obtain carbon fiber-cordierite glass-ceramic composite diphase material.
The preparation method of carbon fiber of the invention-cordierite glass-ceramic composite diphase material, is realized using nitrogen injection
Carbon fiber being uniformly distributed in molten bath, the parent glass for obtaining is combined closely with carbon fiber, simultaneously because by plus
Enter the thermal coefficient of expansion that a certain amount of regulator have adjusted parent glass, thus parent glass during nucleus crystallization is heated with
The similar thermal expansion coefficient of carbon fiber, it is to avoid produce larger stress to cause parent glass brilliant because thermal coefficient of expansion is inconsistent
The phenomenon ftractureed during change.
Referring to specific embodiment, the present invention will be described.
Embodiment one
Reference picture 1, in the step s 100, by the MgO powder of 18 weight portions, the SiO of 50 weight portions2Powder, 10 weight portions
Al2O3The flux B of powder, 3 weight portions2O3, be respectively 2 weight portions Nucleating Agent Cr2O3And P2O5And altogether be 6 weight portions
Regulator Na2O and BaO is well mixed, and obtains preparing the primary raw material of cordierite glass-ceramic.Then in step s 200,
Above-mentioned raw materials are melted into 4 hours at 1560 DEG C, to ensure that raw material is fully melted.Then in the melt stage end of step S200
Phase, according to shown in step S300, by the powder formed carbon fiber of 9 weight portions is by nitrogen stream penetrating bath and is fully stirred
Mix, carbon fiber is uniformly distributed in fused raw material so as to obtain the fused raw material containing equally distributed carbon fiber.Then exist
Step S400, among the fused raw material cast of the carbon fiber-containing that step S300 is obtained enters through 590 DEG C of moulds being fully warmed-up,
And annealed 3 hours at a temperature of 590 DEG C, obtain the parent glass of carbon fiber-containing.Then in step S500, by carbon fiber-containing
Parent glass at a temperature of 640 DEG C coring 2 hours, then at a temperature of 870 DEG C crystallization to obtain within 4 hours carbon fiber-violet blue or green
Stone glass ceramic composite.
Embodiment two
Reference picture 1, in the step s 100, by the MgO powder of 18 weight portions, the SiO of 49 weight portions2Powder, 10 weight portions
Al2O3The flux B of powder, 2 weight portions2O3, be respectively the Nucleating Agent Cr of 2 weight portions and 1 weight portion2O3And P2O5And altogether
It is the regulator Na of 5 weight portions2O and BaO is well mixed, and obtains preparing the primary raw material of cordierite glass-ceramic.Then in step
In rapid S200, above-mentioned raw materials are melted into 4 hours at 1550 DEG C, to ensure that raw material is fully melted.Then step S200's
In melt stage latter stage, according to shown in step S300, the powder formed carbon fiber of 15 weight portions is sprayed into bath by nitrogen stream
And be sufficiently stirred for, carbon fiber is uniformly distributed in fused raw material so as to obtain the melting containing equally distributed carbon fiber
Raw material.Then in step S400, the fused raw material of the carbon fiber-containing that step S300 is obtained is poured into a mould to enter and is fully warmed-up through 590 DEG C
Mould among, and at a temperature of 590 DEG C anneal 3 hours, obtain the parent glass of carbon fiber-containing.Then in step S500
In, by the parent glass of carbon fiber-containing at a temperature of 650 DEG C coring 2 hours, then the crystallization 3 hours at a temperature of 880 DEG C
To carbon fiber-cordierite glass-ceramic composite.
Embodiment three
Reference picture 1, in the step s 100, by the MgO powder of 20 weight portions, the SiO of 60 weight portions2Powder, 24 weight portions
Al2O3The flux B of powder, 5 weight portions2O3, be respectively the Nucleating Agent Cr of 2 weight portions and 3 weight portions2O3And P2O5And altogether
It is the regulator Na of 4 weight portions2O and BaO is well mixed, and obtains preparing the primary raw material of cordierite glass-ceramic.Then in step
In rapid S200, above-mentioned raw materials are melted into 6 hours at 1500 DEG C, to ensure that raw material is fully melted.Then step S200's
In melt stage latter stage, according to shown in step S300, the powder formed carbon fiber of 8 weight portions is sprayed into bath simultaneously by nitrogen stream
It is sufficiently stirred for, carbon fiber is uniformly distributed in fused raw material former so as to obtain the melting containing equally distributed carbon fiber
Material.Then in step S400, the fused raw material of the carbon fiber-containing that step S300 is obtained cast enters and is fully warmed-up through 600 DEG C
Among mould, and annealed 3 hours at a temperature of 600 DEG C, obtain the parent glass of carbon fiber-containing.Then in step S500,
By the parent glass of carbon fiber-containing at a temperature of 600 DEG C coring 3 hours, then crystallization obtains carbon in 6 hours at a temperature of 900 DEG C
Fiber-cordierite glass-ceramic composite.
Example IV
Reference picture 1, in the step s 100, by the MgO powder of 26 weight portions, the SiO of 48 weight portions2Powder, 20 weight portions
Al2O3The flux B of powder, 6 weight portions2O3, be respectively the Nucleating Agent Cr of 1 weight portion and 2 weight portions2O3And P2O5And altogether
It is the regulator Na of 8 weight portions2O and BaO is well mixed, and obtains preparing the primary raw material of cordierite glass-ceramic.Then in step
In rapid S200, above-mentioned raw materials are melted into 3 hours at 1600 DEG C, to ensure that raw material is fully melted.Then step S200's
In melt stage latter stage, according to shown in step S300, the powder formed carbon fiber of 10 weight portions is sprayed into bath by nitrogen stream
And be sufficiently stirred for, carbon fiber is uniformly distributed in fused raw material so as to obtain the melting containing equally distributed carbon fiber
Raw material.Then in step S400, the fused raw material of the carbon fiber-containing that step S300 is obtained is poured into a mould to enter and is fully warmed-up through 650 DEG C
Mould among, and at a temperature of 650 DEG C anneal 6 hours, obtain the parent glass of carbon fiber-containing.Then in step S500
In, by the parent glass of carbon fiber-containing at a temperature of 750 DEG C coring 3 hours, then the crystallization 5 hours at a temperature of 850 DEG C
To carbon fiber-cordierite glass-ceramic composite.
Embodiment five
Reference picture 1, in the step s 100, by the MgO powder of 22 weight portions, the SiO of 50 weight portions2Powder, 15 weight portions
Al2O3The flux B of powder, 4 weight portions2O3, be respectively 2 weight portions Nucleating Agent Cr2O3And P2O5And altogether be 6 weight portions
Regulator Na2O and BaO is well mixed, and obtains preparing the primary raw material of cordierite glass-ceramic.Then in step s 200,
Above-mentioned raw materials are melted into 3 hours at 1650 DEG C, to ensure that raw material is fully melted.Then in the melt stage end of step S200
Phase, according to shown in step S300, by the powder formed carbon fiber of 12 weight portions is by nitrogen stream penetrating bath and carries out fully
Stirring, makes carbon fiber be uniformly distributed in fused raw material so as to obtain the fused raw material containing equally distributed carbon fiber.Then
In step S400, the cast of the fused raw material of the carbon fiber-containing that step S300 is obtained enter through 620 DEG C of moulds being fully warmed-up it
In, and annealed 5 hours at a temperature of 620 DEG C, obtain the parent glass of carbon fiber-containing.Then in step S500, will be carbon containing
The parent glass of fiber coring 3 hours at a temperature of 720 DEG C, then at a temperature of 920 DEG C crystallization obtain within 6 hours carbon fiber-
Cordierite glass-ceramic 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 (10)
1. the preparation method of a kind of carbon fiber-cordierite glass-ceramic composite diphase material, it is characterised in that comprise the steps of：
1) by MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent, regulator are mixed in proportion, and are obtained
Mixed material；
2) by step 1) in obtain mixed material melting heating；
3) in step 2) in melting process latter stage by gas stream by carbon fiber spray into fusion pool in and stir, obtain
To the fused raw material containing carbon fiber；
4) by step 3) in the fused raw material containing carbon fiber that obtains be poured into by the mould that preheats and by annealing
To the parent glass containing carbon fiber；
5) by step 4) in the parent glass coring containing carbon fiber that obtains and crystallization, obtain carbon fiber-cordierite crystallite glass
Glass composite diphase material.
2. the preparation method of carbon fiber according to claim 1-cordierite glass-ceramic composite diphase material, it is characterised in that
The step 1) in the ratio of each powder be：MgO 18-26 weight portions, SiO248-60 weight portions, Al2O310-24 weight portions.
3. the preparation method of carbon fiber according to claim 1-cordierite glass-ceramic composite diphase material, it is characterised in that
The flux is B2O3, the Nucleating Agent is Cr2O3And P2O5, the regulator is Na2O and BaO.
4. the preparation method of carbon fiber according to claim 3-cordierite glass-ceramic composite diphase material, it is characterised in that
The B2O3Ratio be 2-6 weight portions, the Cr2O3And P2O5Ratio be respectively 1-3 weight portions, the Na2O's and BaO
Ratio is altogether 4-8 weight portions.
5. the preparation method of carbon fiber according to claim 1-cordierite glass-ceramic composite diphase material, it is characterised in that
The step 3) in the carbon fiber that adds for powdered.
6. the preparation method of carbon fiber according to claim 5-cordierite glass-ceramic composite diphase material, it is characterised in that
The ratio of the carbon fiber is 8-15 weight portions.
7. the preparation method of carbon fiber according to claim 1-cordierite glass-ceramic composite diphase material, it is characterised in that
The step 2) in gas stream be nitrogen stream.
8. the preparation method of carbon fiber according to claim 1-cordierite glass-ceramic composite diphase material, it is characterised in that
The step 2) in melting heating carried out at a temperature of 1480-1650 DEG C, the step 4) in the preheating temperature of mould be
450-650 DEG C, annealing temperature be 450-650 DEG C, the step 5) in nucleation temperature for 550-750 DEG C, crystallization temperature be
750-980℃。
9. the preparation method of carbon fiber according to claim 1-cordierite glass-ceramic composite diphase material, it is characterised in that
The step 2) in the melting heat time be 3-6 hour, the step 4) in annealing time be 4-8 hours, the step
5) nucleation time in is 2-3 hours, crystallization time is 4-8 hours.
10. a kind of preparation using carbon fiber as claimed in any one of claims 1-9 wherein-cordierite glass-ceramic composite diphase material
Carbon fiber-cordierite glass-ceramic composite diphase material prepared by method.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59232924A (en) * | 1983-06-15 | 1984-12-27 | Semiconductor Energy Lab Co Ltd | Manufacture of glass sheet |
| CN101423332A (en) * | 2008-10-17 | 2009-05-06 | 韦鸿雁 | Technique for adding fiberglass or other fibre to glass |
| CN101475299A (en) * | 2008-12-03 | 2009-07-08 | 中国兵器工业集团第五三研究所 | Technique of preparing fiber reinforcement glass based composite material |
| CN104496186A (en) * | 2014-12-31 | 2015-04-08 | 海南大学 | Cordierite-based nanometer glass-ceramic and preparation method thereof |
-
2016
- 2016-12-21 CN CN201611192282.5A patent/CN106698956A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59232924A (en) * | 1983-06-15 | 1984-12-27 | Semiconductor Energy Lab Co Ltd | Manufacture of glass sheet |
| CN101423332A (en) * | 2008-10-17 | 2009-05-06 | 韦鸿雁 | Technique for adding fiberglass or other fibre to glass |
| CN101475299A (en) * | 2008-12-03 | 2009-07-08 | 中国兵器工业集团第五三研究所 | Technique of preparing fiber reinforcement glass based composite material |
| CN104496186A (en) * | 2014-12-31 | 2015-04-08 | 海南大学 | Cordierite-based nanometer glass-ceramic and preparation method thereof |
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