CN106746694A - A kind of carbon fiber diopside devitrified glass composite diphase material and preparation method thereof - Google Patents
A kind of carbon fiber diopside devitrified glass composite diphase material and preparation method thereof Download PDFInfo
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- CN106746694A CN106746694A CN201611191364.8A CN201611191364A CN106746694A CN 106746694 A CN106746694 A CN 106746694A CN 201611191364 A CN201611191364 A CN 201611191364A CN 106746694 A CN106746694 A CN 106746694A
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- carbon fiber
- diopside
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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
- 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
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The present invention relates to a kind of preparation method of carbon fiber diopside devitrified glass composite diphase material, it is comprised the steps of：By CaO powder, MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent, regulator are mixed in proportion, and obtain mixed material；The mixed material melting that will be obtained is heated and carbon fiber is sprayed into fusion pool and stirred by gas stream in the latter stage of melting process, obtains the fused raw material containing carbon fiber；The fused raw material containing carbon fiber that will be obtained is poured into the mould by preheating and obtains the parent glass containing carbon fiber by annealing；The parent glass coring containing carbon fiber that will be obtained and crystallization, obtain carbon fiber diopside devitrified glass composite diphase material.The present invention have effectively achieved the efficient preparation of carbon fiber diopside devitrified glass composite diphase material by the preparation method.
Description
Technical field
The present invention relates to glass ceramic composite field, more particularly, to a kind of carbon fiber-diopside devitrified glass
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 diopside devitrified glass using fusion method in current there is no in the prior art, is prepared
The report of carbon fiber-diopside devitrified glass 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-diopside devitrified glass 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-diopside devitrified glass composite diphase material,
Comprise the steps of：
1) by CaO powder, MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent, regulator are mixed in proportion
Close uniform, 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-diopside micro-
Crystal glass composite diphase material.
According to one embodiment of present invention, above-mentioned steps 1) in the ratio of each powder be：CaO 12-20 weight portions, MgO
8-15 weight portions, SiO244-56 weight portions, Al2O36-12 weight portions.
According to one embodiment of present invention, flux is CaF in above-mentioned steps2, Nucleating Agent is P2O5And TiO2, regulator
It is MgO.
According to one embodiment of present invention, CaF2Ratio be 1-4 weight portions, P2O5And TiO2Ratio be respectively 2-5
Weight portion, the ratio of MgO is 5-10 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 12-18 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 1400-1600 DEG C,
Step 4) in mould preheating temperature for 400-600 DEG C, annealing temperature be 400-600 DEG C, step 5) in nucleation temperature be
500-700 DEG C, crystallization temperature be 700-900 DEG C.
According to one embodiment of present invention, above-mentioned steps 2) in the melting heat time be 2-6 hours, step 4) in
Annealing time be 2-5 hour, step 5) in nucleation time for 4-8 hours, crystallization time be 4-8 hours.
By the above method, the efficient preparation of carbon fiber-diopside devitrified glass composite diphase material is have effectively achieved.
According to another aspect of the present invention, a kind of carbon fiber-diopside using the preparation of above-mentioned preparation method is also provided micro-
Crystal glass composite diphase material.
There is carbon fiber-diopside devitrified glass composite diphase material prepared by the present invention porosity to be far below sintering process crystallite glass
The features such as glass, carbon fiber and substrate glass are tightly combined, toughness of material is greatly improved.
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-diopside devitrified glass 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-diopside devitrified glass composite diphase material.Reference picture 1, the preparation
Method is comprised the following steps：
S100 mixes in proportion
In the present invention, by CaO powder, MgO powder, SiO2Powder, Al2O3Powder, flux CaF2, Nucleating Agent P2O5With
TiO2, regulator MgO mix in proportion, obtain preparing the primary raw material of diopside devitrified glass.Wherein above-mentioned each component
Ratio be CaO 12-20 weight portions, MgO 8-15 weight portions, SiO244-56 weight portions, Al2O3It is 6-12 weight portions, fluxing
Agent CaF21-4 weight portions, Nucleating Agent P2O52-5 weight portions and TiO22-5 weight portions, regulator MgO 5-10 weight portions, powder
The particle diameter at end is less than 200 mesh.
S200 is fully melted
In the present invention, the primary raw material for preparing diopside devitrified glass that will be obtained in S100 is molten at 1400-1600 DEG C
Melt heating 2-6 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 12-18 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 400-600 DEG C preheating mould in simultaneously
Annealing 2-5 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 4-8 hours at 500-700 DEG C, then it is warming up to 700-
900 DEG C crystallization 4-8 hours, and then obtain carbon fiber-diopside devitrified glass composite diphase material.
The preparation method of carbon fiber of the invention-diopside devitrified glass 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 CaO powder of 12 weight portions, the MgO powder of 10 weight portions, 46 weight portions
SiO2The Al of powder, 6 weight portions2O3The flux CaF of powder, 2 weight portions2, be respectively 2 weight portions Nucleating Agent P2O5And TiO2
And 6 weight portion regulator MgO be well mixed, obtain preparing the primary raw material of diopside devitrified glass.Then in step
In S200, above-mentioned raw materials are melted into 3 hours at 1550 DEG C, to ensure that raw material is fully melted.Then in the molten of step S200
Melt latter stage in stage, according to shown in step S300, the powder formed carbon fiber of 14 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 550 DEG C
Among mould, and annealed 3 hours at a temperature of 550 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 650 DEG C coring 2 hours, then crystallization obtains carbon in 4 hours at a temperature of 850 DEG C
Fiber diopside glass ceramic composite.
Embodiment two
Reference picture 1, in the step s 100, by the CaO powder of 14 weight portions, the MgO powder of 9 weight portions, 45 weight portions
SiO2The Al of powder, 6 weight portions2O3The flux CaF of powder, 2 weight portions2, be respectively 2 weight portions Nucleating Agent P2O5And TiO2
And 8 weight portion regulator MgO be well mixed, obtain preparing the primary raw material of diopside devitrified glass.Then in step
In S200, above-mentioned raw materials are melted into 4 hours at 1560 DEG C, to ensure that raw material is fully melted.Then in the molten of step S200
Melt latter stage in stage, according to shown in step S300, the powder formed carbon fiber of 12 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 580 DEG C
Among mould, and annealed 2 hours at a temperature of 580 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 630 DEG C coring 2 hours, then crystallization obtains carbon in 4 hours at a temperature of 830 DEG C
Fiber diopside glass ceramic composite.
Embodiment three
Reference picture 1, in the step s 100, by the CaO powder of 20 weight portions, the MgO powder of 10 weight portions, 44 weight portions
SiO2The Al of powder, 10 weight portions2O3The flux CaF of powder, 4 weight portions2, be respectively the nucleus of 2 weight portions and 5 weight portions
Agent P2O5And TiO2And 6 weight portion regulator MgO be well mixed, obtain preparing the primary raw material of diopside devitrified glass.With
Afterwards in step s 200, above-mentioned raw materials are melted into 6 hours at 1600 DEG C, to ensure that raw material is fully melted.Then in step
In the melt stage latter stage of S200, according to shown in step S300, the powder formed carbon fiber of 15 weight portions is sprayed into by nitrogen stream molten
Pond inside is simultaneously sufficiently stirred for, and carbon fiber is uniformly distributed in fused raw material so as to obtain containing equally distributed carbon fiber
Fused raw material.Then in step S400, the fused raw material cast of the carbon fiber-containing that step S300 is obtained enters fills through 600 DEG C
Divide among the mould of preheating, and annealed 4 hours at a temperature of 600 DEG C, obtain the parent glass of carbon fiber-containing.Then in step
In S500, by the parent glass of carbon fiber-containing at a temperature of 500 DEG C coring 4 hours, then crystallization 6 is small at a temperature of 700 DEG C
When obtain carbon fiber diopside glass ceramic composite.
Example IV
Reference picture 1, in the step s 100, by the CaO powder of 20 weight portions, the MgO powder of 15 weight portions, 56 weight portions
SiO2The Al of powder, 9 weight portions2O3The flux CaF of powder, 1 weight portion2, be respectively the Nucleating Agent of 5 weight portions and 2 weight portions
P2O5And TiO2And 9 weight portion regulator MgO be well mixed, obtain preparing the primary raw material of diopside devitrified glass.Then
In step s 200, above-mentioned raw materials are melted into 2 hours at 1560 DEG C, to ensure that raw material is fully melted.Then in step
In the melt stage latter stage of S200, according to shown in step S300, the powder formed carbon fiber of 18 weight portions is sprayed into by nitrogen stream molten
Pond inside is simultaneously sufficiently stirred for, and carbon fiber is uniformly distributed in fused raw material so as to obtain containing equally distributed carbon fiber
Fused raw material.Then in step S400, the fused raw material cast of the carbon fiber-containing that step S300 is obtained enters fills through 550 DEG C
Divide among the mould of preheating, and annealed 4 hours at a temperature of 550 DEG C, obtain the parent glass of carbon fiber-containing.Then in step
In S500, by the parent glass of carbon fiber-containing at a temperature of 500 DEG C coring 8 hours, then crystallization 4 is small at a temperature of 820 DEG C
When obtain carbon fiber diopside glass ceramic composite.
Embodiment five
Reference picture 1, in the step s 100, by the CaO powder of 18 weight portions, the MgO powder of 8 weight portions, 56 weight portions
SiO2The Al of powder, 12 weight portions2O3The flux CaF of powder, 3 weight portions2, be respectively the nucleus of 2 weight portions and 3 weight portions
Agent P2O5And TiO2And 10 weight portion regulator MgO be well mixed, obtain preparing the primary raw material of diopside devitrified glass.
Then in step s 200, above-mentioned raw materials are melted into 6 hours at 1480 DEG C, to ensure that raw material is fully melted.Then in step
In the melt stage latter stage of rapid S200, according to shown in step S300, the powder formed carbon fiber of 16 weight portions is sprayed into by nitrogen stream
Bath is simultaneously sufficiently stirred for, and carbon fiber is uniformly distributed in fused raw material fine containing equally distributed carbon so as to obtain
The fused raw material of dimension.Then in step S400, the fused raw material cast of the carbon fiber-containing that step S300 is obtained enters through 520 DEG C
Among the mould being fully warmed-up, and annealed 5 hours at a temperature of 520 DEG C, obtain the parent glass of carbon fiber-containing.Then in step
In rapid S500, by the parent glass of carbon fiber-containing at a temperature of 700 DEG C coring 3 hours, then the crystallization 8 at a temperature of 900 DEG C
Hour obtains carbon fiber diopside 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-diopside devitrified glass composite diphase material, it is characterised in that comprise the steps of：
1) by CaO powder, MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent, regulator mix in proportion
It is even, 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 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-diopside crystallite glass
Glass composite diphase material.
2. the preparation method of carbon fiber according to claim 1-diopside devitrified glass composite diphase material, it is characterised in that
The step 1) in the ratio of each powder be：CaO 12-20 weight portions, MgO 8-15 weight portions, SiO244-56 weight portions,
Al2O36-12 weight portions.
3. the preparation method of carbon fiber according to claim 1-diopside devitrified glass composite diphase material, it is characterised in that
The flux is CaF2, the Nucleating Agent is P2O5And TiO2, the regulator is MgO.
4. the preparation method of carbon fiber according to claim 3-diopside devitrified glass composite diphase material, it is characterised in that
The CaF2Ratio be 1-4 weight portions, the P2O5And TiO2Ratio be respectively 2-5 weight portions, the ratio of the MgO is
5-10 weight portions.
5. the preparation method of carbon fiber according to claim 1-diopside devitrified glass 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-diopside devitrified glass composite diphase material, it is characterised in that
The ratio of the carbon fiber is 12-18 weight portions.
7. the preparation method of carbon fiber according to claim 1-diopside devitrified glass 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-diopside devitrified glass composite diphase material, it is characterised in that
The step 2) in melting heating carried out at a temperature of 1400-1600 DEG C, the step 4) in the preheating temperature of mould be
400-600 DEG C, annealing temperature be 400-600 DEG C, the step 5) in nucleation temperature for 500-700 DEG C, crystallization temperature be
700-900℃。
9. the preparation method of carbon fiber according to claim 1-diopside devitrified glass composite diphase material, it is characterised in that
The step 2) in the melting heat time be 2-6 hour, the step 4) in annealing time be 2-5 hours, the step
5) nucleation time in is 4-8 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-diopside devitrified glass composite diphase material
Carbon fiber-diopside devitrified glass composite diphase material prepared by method.
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