CN106854041A - A kind of carbon fiber wollastonite devitrified glass composite diphase material and preparation method thereof - Google Patents

A kind of carbon fiber wollastonite devitrified glass composite diphase material and preparation method thereof Download PDF

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Publication number
CN106854041A
CN106854041A CN201611192237.XA CN201611192237A CN106854041A CN 106854041 A CN106854041 A CN 106854041A CN 201611192237 A CN201611192237 A CN 201611192237A CN 106854041 A CN106854041 A CN 106854041A
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China
Prior art keywords
carbon fiber
preparation
glass composite
devitrified glass
composite diphase
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CN201611192237.XA
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Chinese (zh)
Inventor
马冬阳
边妙莲
孙辉
陈士朝
吴道洪
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Jiangsu Province Metallurgical Design Institute Co Ltd
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Jiangsu Province Metallurgical Design Institute Co Ltd
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Priority to CN201611192237.XA priority Critical patent/CN106854041A/en
Publication of CN106854041A publication Critical patent/CN106854041A/en
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C14/00Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/002Glass 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
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00Thermal 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
    • C03B32/02Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C10/00Devitrified 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
    • C03C10/0009Devitrified 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

Abstract

The present invention relates to a kind of preparation method of carbon fiber wollastonite devitrified glass composite diphase material, it is comprised the steps of:By CaO 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 wollastonite devitrified glass composite diphase material.The present invention have effectively achieved the efficient preparation of carbon fiber wollastonite devitrified glass composite diphase material by the preparation method.

Description

A kind of carbon fiber-wollastonite devitrified glass composite diphase material and preparation method thereof
Technical field
The present invention relates to glass ceramic composite field, more particularly, to a kind of carbon fiber-wollastonite 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 wollastonite devitrified glass using fusion method in current there is no in the prior art, is prepared The report of carbon fiber-wollastonite 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-wollastonite 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-wollastonite devitrified glass composite diphase material, Comprise the steps of:
1) by CaO 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-wollastonite 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 12-16 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 Cr2O3And TiO2, adjustment Agent is MgO.
According to one embodiment of present invention, CaF2Ratio be 2-6 weight portions, Cr2O3And TiO2Ratio be respectively 1-3 Weight portion, the ratio of MgO is 6-12 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 15-20 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 1430-1600 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 530-730 DEG C, crystallization temperature be 730-930 DEG C.
According to one embodiment of present invention, above-mentioned steps 2) in the melting heat time be 2-5 hours, the step 4) In annealing time be 2-5 hour, step 5) in nucleation time for 2-3 hours, crystallization time be 2-4 hours.
The present invention have effectively achieved the efficient system of carbon fiber-wollastonite devitrified glass composite diphase material by the above method It is standby.
According to another aspect of the present invention, a kind of carbon fiber-wollastonite using the preparation of above-mentioned preparation method is also provided micro- Crystal glass composite diphase material.
The present invention prepare carbon fiber-wollastonite microcrystal glass 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-wollastonite 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-wollastonite 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, SiO2Powder, Al2O3Powder, flux CaF2, Nucleating Agent Cr2O3With TiO2, adjust Whole dose of MgO is mixed in proportion, and obtains preparing the primary raw material of wollastonite devitrified glass.The ratio of wherein above-mentioned each component is CaO 12-16 weight portions, SiO244-56 weight portions, Al2O36-12 weight portions, flux CaF22-6 weight portions, Nucleating Agent Cr2O31-3 weight portions and TiO21-3 weight portions, regulator MgO 6-12 weight portions, the particle diameter of powder are less than 200 mesh.
S200 is fully melted
In the present invention, the primary raw material for preparing wollastonite devitrified glass that will be obtained in S100 is molten at 1430-1600 DEG C Melt heating 2-5 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 15-20 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 Lower the temperature with stove again after annealing 2-5 as a child at 400-600 DEG C, obtain 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 530-730 DEG C, then it is warming up to 730- 930 DEG C crystallization 2-4 hours, and then obtain carbon fiber-wollastonite devitrified glass composite diphase material.
The preparation method of carbon fiber of the invention-wollastonite 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 SiO of 46 weight portions2Powder, 10 weight portions Al2O3The flux CaF of powder, 3 weight portions2, be respectively 2 weight portions Nucleating Agent Cr2O3And TiO2And 10 weight portions Regulator MgO is well mixed, and obtains preparing the primary raw material of wollastonite devitrified glass.Then in step s 200, by above-mentioned original Material melts 4 hours at 1530 DEG C, to ensure that raw material is fully melted.Then in the melt stage latter stage of step S200, according to Shown in step S300, by the powder formed carbon fiber of 15 weight portions is by nitrogen stream penetrating bath and is sufficiently stirred for, make Carbon fiber is uniformly distributed in fused raw material so as to obtain the fused raw material containing equally distributed carbon fiber.Then in step S400, among the fused raw material cast of the carbon fiber-containing that step S300 is obtained enters through 580 DEG C of moulds being fully warmed-up, 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 base of carbon fiber-containing Plinth glass coring 2 hours at a temperature of 660 DEG C, then at a temperature of 860 DEG C crystallization to obtain carbon fiber-wollastonite within 4 hours micro- Crystal glass composite.
Embodiment two
Reference picture 1, in the step s 100, by the CaO powder of 15 weight portions, the SiO of 50 weight portions2Powder, 6 weight portions Al2O3The flux CaF of powder, 2 weight portions2, be respectively 2 weight portions Nucleating Agent Cr2O3And TiO2And 7 weight portion adjustment Agent MgO is well mixed, and obtains preparing the primary raw material of wollastonite devitrified glass.Then in step s 200, above-mentioned raw materials are existed 4 hours are melted at 1550 DEG C, to ensure that raw material is fully melted.Then in the melt stage latter stage of step S200, according to step Shown in S300, by the powder formed carbon fiber of 15 weight portions is by nitrogen stream penetrating bath and is sufficiently stirred for, make carbon fine Dimension is uniformly distributed in fused raw material so as to obtain the fused raw material containing equally distributed carbon fiber.Then in step S400, Among the fused raw material cast of the carbon fiber-containing that step S300 is obtained enters through 560 DEG C of moulds being fully warmed-up, and at 560 DEG C At a temperature of anneal 2 hours, obtain the parent glass of carbon fiber-containing.Then in step S500, by the basic glass of carbon fiber-containing Glass coring 2 hours at a temperature of 650 DEG C, then crystallization obtains carbon fiber-wollastonite crystallite glass for 3 hours at a temperature of 850 DEG C Glass composite.
Embodiment three
Reference picture 1, in the step s 100, by the CaO powder of 16 weight portions, the SiO of 56 weight portions2Powder, 12 weight portions Al2O3The flux CaF of powder, 4 weight portions2, be respectively 3 weight portions Nucleating Agent Cr2O3And TiO2And 6 weight portion tune Whole dose of MgO is well mixed, and obtains preparing the primary raw material of wollastonite devitrified glass.Then in step s 200, by above-mentioned raw materials 3 hours are melted at 1580 DEG C, to ensure that raw material is fully melted.Then in the melt stage latter stage of step S200, according to step Shown in rapid S300, by the powder formed carbon fiber of 18 weight portions is by nitrogen stream penetrating bath and is sufficiently stirred for, make carbon Fiber is uniformly distributed in fused raw material so as to obtain the fused raw material containing equally distributed carbon fiber.Then in step S400, among the fused raw material cast of the carbon fiber-containing that step S300 is obtained enters through 600 DEG C of moulds being fully warmed-up, 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 base of carbon fiber-containing Plinth glass coring 2 hours at a temperature of 700 DEG C, then at a temperature of 800 DEG C crystallization to obtain carbon fiber-wollastonite within 3 hours micro- Crystal glass composite.
Example IV
Reference picture 1, in the step s 100, by the CaO powder of 16 weight portions, the SiO of 44 weight portions2Powder, 10 weight portions Al2O3The flux CaF of powder, 6 weight portions2, be respectively the Nucleating Agent Cr of 1 weight portion and 2 weight portions2O3And TiO2And 10 The regulator MgO of weight portion is well mixed, and obtains preparing the primary raw material of wollastonite devitrified glass.Then in step s 200, Above-mentioned raw materials are melted into 2 hours at 1600 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 20 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 580 DEG C of moulds being fully warmed-up it In, and annealed 4 hours at a temperature of 580 DEG C, obtain the parent glass of carbon fiber-containing.Then in step S500, will be carbon containing The parent glass of fiber coring 2 hours at a temperature of 730 DEG C, then at a temperature of 830 DEG C crystallization obtain within 4 hours carbon fiber- Wollastonite glass ceramic composite.
Embodiment five
Reference picture 1, in the step s 100, by the CaO powder of 15 weight portions, the SiO of 50 weight portions2Powder, 10 weight portions Al2O3The flux CaF of powder, 5 weight portions2, be respectively the Nucleating Agent Cr of 3 weight portions and 2 weight portions2O3And TiO2And 10 The regulator MgO of weight portion is well mixed, and obtains preparing the primary raw material of wollastonite devitrified glass.Then in step s 200, Above-mentioned raw materials are melted into 4 hours at 1500 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 17 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 500 DEG C of moulds being fully warmed-up it In, and annealed 5 hours at a temperature of 500 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 700 DEG C, then crystallization obtains carbon fiber in 2 hours at a temperature of 900 DEG C Silicon-lime stone 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-wollastonite devitrified glass composite diphase material, it is characterised in that comprise the steps of:
1) by CaO 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-wollastonite crystallite glass Glass composite diphase material.
2. the preparation method of carbon fiber according to claim 1-wollastonite devitrified glass composite diphase material, it is characterised in that The step 1) in the ratio of each powder be:CaO 12-16 weight portions, SiO244-56 weight portions, Al2O36-12 weight portions.
3. the preparation method of carbon fiber according to claim 1-wollastonite devitrified glass composite diphase material, it is characterised in that The flux is CaF2, the Nucleating Agent is Cr2O3And TiO2, the regulator is MgO.
4. the preparation method of carbon fiber according to claim 3-wollastonite devitrified glass composite diphase material, it is characterised in that The CaF2Ratio be 2-6 weight portions, the Cr2O3And TiO2Ratio be respectively 1-3 weight portions, the ratio of the MgO is 6-12 weight portions.
5. the preparation method of carbon fiber according to claim 1-wollastonite 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-wollastonite devitrified glass composite diphase material, it is characterised in that The ratio of the carbon fiber is 15-20 weight portions.
7. the preparation method of carbon fiber according to claim 1-wollastonite 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-wollastonite devitrified glass composite diphase material, it is characterised in that The step 2) in melting heating carried out at a temperature of 1430-1600 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 530-730 DEG C, crystallization temperature be 730-930℃。
9. the preparation method of carbon fiber according to claim 1-wollastonite devitrified glass composite diphase material, it is characterised in that The step 2) in the melting heat time be 2-5 hour, the step 4) in annealing time be 2-5 hours, the step 5) nucleation time in is 2-3 hours, crystallization time is 2-4 hours.
10. a kind of preparation using carbon fiber as claimed in any one of claims 1-9 wherein-wollastonite devitrified glass composite diphase material Carbon fiber-wollastonite devitrified glass composite diphase material prepared by method.
CN201611192237.XA 2016-12-21 2016-12-21 A kind of carbon fiber wollastonite devitrified glass composite diphase material and preparation method thereof Pending CN106854041A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114436671A (en) * 2022-01-28 2022-05-06 烟台大学 Foam ceramic-based interference type wave-absorbing material and preparation method thereof

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JPH0375241A (en) * 1989-08-11 1991-03-29 Tokyo Metropolis Production of crystallized glass
CN1066834A (en) * 1991-05-20 1992-12-09 中国科学院上海硅酸盐研究所 The manufacture method of white series microlith glass high grade building material
CN1101027A (en) * 1993-09-29 1995-04-05 中国建筑材料科学研究院 Technology for production of fiber reinforced glass and glass-ceramic base composite material
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JPH0375241A (en) * 1989-08-11 1991-03-29 Tokyo Metropolis Production of crystallized glass
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Publication number Priority date Publication date Assignee Title
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CN114436671B (en) * 2022-01-28 2023-03-14 烟台大学 Foam ceramic-based interference type wave-absorbing material and preparation method thereof

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