CN106966744A - A kind of fibre reinforced alumina ceramic composite material and preparation method thereof - Google Patents

A kind of fibre reinforced alumina ceramic composite material and preparation method thereof Download PDF

Info

Publication number
CN106966744A
CN106966744A CN201610391203.7A CN201610391203A CN106966744A CN 106966744 A CN106966744 A CN 106966744A CN 201610391203 A CN201610391203 A CN 201610391203A CN 106966744 A CN106966744 A CN 106966744A
Authority
CN
China
Prior art keywords
fibre reinforced
composite material
ceramic composite
preparation
alumina ceramic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201610391203.7A
Other languages
Chinese (zh)
Other versions
CN106966744B (en
Inventor
罗瑞盈
李小孟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beihang University
Original Assignee
Beihang University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beihang University filed Critical Beihang University
Priority to CN201610391203.7A priority Critical patent/CN106966744B/en
Publication of CN106966744A publication Critical patent/CN106966744A/en
Application granted granted Critical
Publication of CN106966744B publication Critical patent/CN106966744B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C04B35/803
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/624Sol-gel processing
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5053Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
    • C04B41/5057Carbides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/87Ceramics
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/524Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248Carbon, e.g. graphite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/616Liquid infiltration of green bodies or pre-forms

Abstract

The present invention relates to a kind of fibre reinforced alumina ceramic composite material and preparation method thereof.Wherein, the preparation method comprises the following steps:S101:Using Alumina gel as precursor, vacuum impregnation is carried out to carbon felt, then densification will be carried out with the impregnated carbon felt of Alumina gel, to prepare the aluminium oxide ceramics of fibre reinforced;S102:Vacuum impregnation is carried out to the aluminium oxide ceramics of fibre reinforced using sol-gal process, then dries, sinters, and is cooled to room temperature, to prepare Si Al C coatings.According to a kind of preparation method of fibre reinforced alumina ceramic composite material of the present invention, its short preparation period and cost is low;According to a kind of fibre reinforced alumina ceramic composite material of the present invention, its mechanical property, resistance to elevated temperatures are excellent.

Description

A kind of fibre reinforced alumina ceramic composite material and preparation method thereof
Technical field
The present invention relates to Material Field, and in particular to a kind of fibre reinforced alumina ceramic composite material and its preparation side Method.
Background technology
Aluminium oxide ceramics has the advantages that fusing point height, good stability at elevated temperature, modulus and intensity are higher, can be in high temperature Used for a long time in oxidation environment.But bulk oxidation aluminium ceramics toughness is typically relatively low, easily occurs catastrophic failure, limits Its application in engineering structure.To improve the mechanical property of aluminium oxide ceramics, various toughening mechanisms are widely used, main bag Include the modes such as particle enhancing, whisker reinforcement and fiber reinforcement, wherein particle and crystal whisker toughened can significantly improve aluminium oxide ceramics Intensity, but relatively low is improved to its toughness, and particle and crystal whisker toughened aluminum oxide ceramics use heat pressing process more, it is difficult to it is molded large-scale Complexity is built.It is considered as that the promising improvement ceramics of comparison are tough to carry out toughening ceramic using the fiber of high-modulus, high intensity at present The approach of property.According to composite theory, when Crack Extension is to fiber, energy is absorbed by the disengaging in fiber and matrix section Amount, relaxes stress concentration, and few fibers will also consume a large amount of energy when generation fracture is extracted from matrix under tensile stress is acted on Amount, these are all conducive to strengthening the toughness of ceramic material.
The preparation method of aluminium oxide ceramics has a variety of, and wherein sol-gel process is that the one kind for preparing aluminium oxide ceramics is commonly used Method, it is, at room temperature through hydrolysis, polycondensation, to obtain colloidal sol and gel, then carried out heat by aluminium-alcohol salt or aluminium salt slightly higher Cracking, obtains a kind of method of aluminium oxide ceramics.Outstanding feature of this method in terms of material preparation be:(1) due to gel mistake Cheng Zhong, the size of particle is Nano grade, therefore can substantially reduce sintering temperature;(2) its chemistry can be made in one phase matrix Composition reaches visibly homogeneous;(3) before cracking, by colloidal sol and gel two states, easily fiber and its braid are carried out Dipping and excipient, thus be easy to prepare fibre reinforced composites.
The difference of alumina raw material is prepared according to sol-gal process, the preparation of alumina sol can be divided into organic salt original Material method, inorganic salt raw material method, powder method.Organic salt method is, using aluminium isopropoxide as raw material, to possess stirring, backflow and charging function Device in, Organic Ingredients is added dropwise in water, is stirred vigorously at 80 DEG C, most of alcohol is boiled off, then flows back again a few hours.Nothing Machine salt method is to be dissolved in water by metal salt digestion in hydrochloric acid or aluminium chloride or by pure aluminum nitrate is analyzed, and solution is adjusted with ammoniacal liquor PH.Powder method is to use SB powder (boehmite) or alumina powder, and colloidal sol is obtained by the way that powder is scattered.
Specific strength, specific modulus and the fatigue strength of carbon fiber are high, are a kind of good reinforcement materials, but carbon fiber exists More than 400 DEG C are very easy to aoxidize, and cause the calamitous decline of material property.Silicon carbide fibre is also a kind of increasing well Strong body material, its heat resistance and inoxidizability are superior to carbon fiber, but silicon carbide fibre is very expensive, and which has limited making for it Use scope.Therefore there is important meaning to expanding it using scope solving to minimize cost on the basis of carbon fiber is oxidation resistant Justice.
The content of the invention
It is contemplated that at least solving one of technical problem in correlation technique to a certain extent.
Therefore, it is an object of the present invention to propose that a kind of mechanical property, resistance to elevated temperatures are excellent, and manufacturing cycle A kind of preparation method of the low fibre reinforced alumina ceramic composite material of short, cost.
A kind of preparation method of fibre reinforced alumina ceramic composite material according to embodiments of the present invention, including it is as follows Step:S101:Using Alumina gel as precursor, vacuum impregnation is carried out to carbon felt, then will be carried out with the impregnated carbon felt of Alumina gel Densification, to prepare the aluminium oxide ceramics of fibre reinforced;S102:Oxidation using sol-gal process to fibre reinforced Aluminium ceramics carry out vacuum impregnation, then dry, and sinter, and are cooled to room temperature, to prepare Si-Al-C coatings.
A kind of fibre reinforced alumina ceramic composite material according to embodiments of the present invention, carbon fiber is made pottery as aluminum oxide The reinforcement of porcelain, its specific strength and specific modulus are high, and no creep, fatigue durability is good, and thermal coefficient of expansion is small, corrosion resistance, and oxygen The section wellability for changing Alumina gel and carbon fiber is relatively good, and interface binding power is moderate.Carbon fiber ensure that increasing in the form of carbon felt Strong phase is evenly distributed, it is to avoid the problem of particle enhancing and whisker reinforcement skewness.It is by vacuum impregnation technology that carbon is fine Dimension enhancing alumina ceramic composite material carries out densification, considerably increases the mechanical strength of material.With powder sintering method Prepare aluminium oxide ceramics to compare, preparing aluminium oxide ceramics using sol-gel process can drop to sintering temperature from 1800 DEG C 1300 DEG C, greatly reduce equipment requirement and energy resource consumption.The Si-Al-C antioxidant coatings that the present invention is used are very fine and close, with Alumina substrate is well combined, can effective reinforcing material inoxidizability.
In addition, a kind of preparation side of fibre reinforced alumina ceramic composite material according to the above embodiment of the present invention Method, can also have technical characteristic additional as follows:
Further, in step s 102, vacuum impregnation process is carried out using just to the aluminium oxide ceramics of fibre reinforced Silester base silica sol, nitric acid aluminium base alumina sol and the mixed liquor of egg solution composition.
Further, in step s 102, the preparation of mixed liquor comprises the following steps:Take 30mL~40mL positive silicic acid second With system in the water and alcohol mixeding liquid of ester, 15g~25g aluminum nitrate and a certain amount of hexamethylenetetramine addition 55mL~65mL Standby tetraethyl orthosilicate base silica sol and nitric acid aluminium base alumina sol;To the tetraethyl orthosilicate base silica sol and nitre 100mL~130mL egg clear solution is added in sour aluminium base alumina sol.
Further, in step S101, densif iotacation processing step is specially:It will be dried with the impregnated carbon felt of Alumina gel Afterwards, 1200 DEG C~1400 DEG C are warming up to according to 4 DEG C/min~6 DEG C/min heating rate, then vacuum-sintering 1h~3h cools down To room temperature.
Further, in step S101, precursor be nitric acid Alumina gel, wherein, aluminum ions concentration be 3mol/L~ 4mol/L, the viscosity of Alumina gel is 4mPaS~6mPaS.
Further, in step s 102, sintering temperature is 1200 DEG C~1400 DEG C.
Further, the preparation method of nitric acid Alumina gel comprises the following steps:Excessive aluminum nitrate is added to the water, to make Standby aluminum nitrate solution;Aluminum nitrate solution is heated to 85 DEG C~90 DEG C, after aluminum nitrate is completely dissolved, 10%~15% is added The pH value of ammoniacal liquor to liquid is 3.5~5.0, and then evaporating moisture makes aluminum ions concentration reach after 5mol/L~6mol/L, mistake Filter, takes filtrate, that is, obtains aluminum nitrate colloidal sol.
Another object of the present invention is to propose a kind of fibre reinforced alumina ceramic composite material.
According to a kind of fibre reinforced alumina ceramic composite material of the present invention, including:Reinforcement, reinforcement is carbon Felt;Matrix, matrix is submerged in the space of reinforcement by vacuum impregnation technology, and composite is prepared into reinforcement;Antioxygen Change coating, antioxidant coating is Si-Al-C coatings, and antioxidant coating wraps up the composite.
Further, the density of fibre reinforced alumina ceramic composite material is more than or equal to 2.5g/cm3
Further, carbon felt is PAN based carbon felt.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description Obtain substantially, or recognized by the practice of the present invention.
Brief description of the drawings
Fig. 1 is a kind of preparation method flow chart of fibre reinforced alumina ceramic composite material of the embodiment of the present invention.
Embodiment
Below with reference to the accompanying drawings a kind of preparation side of fibre reinforced alumina ceramic composite material of the present invention is described in detail Method.
As shown in figure 1, a kind of preparation side of fibre reinforced alumina ceramic composite material according to embodiments of the present invention Method, comprises the following steps:
S101:Using Alumina gel as precursor, vacuum impregnation is carried out to carbon felt, then will be entered with the impregnated carbon felt of Alumina gel Row densification, to prepare the aluminium oxide ceramics of fibre reinforced.Specifically, it is right first using nitric acid Alumina gel as precursor Carbon felt after ultrasonic cleaning carries out vacuum impregnation, then re-dry, dries and is put into vacuum-sintering in high temperature furnace after finishing, keeps Vacuum cooled completes a densification process, then repeats the above steps 10~12 times, be until sample no longer increases weight to room temperature Only, with obtained fibre reinforced alumina composite ceramic.Carbon fiber is used as the reinforcement of aluminium oxide ceramics, its specific strength and Bi Mo Amount is high, and no creep, fatigue durability is good, and thermal coefficient of expansion is small, corrosion resistance, and the section infiltration of alumina sol and carbon fiber Property is relatively good, and interface binding power is moderate.Carbon fiber ensure that enhancing phase is evenly distributed in the form of carbon felt, it is to avoid particle increasing The problem of strong and whisker reinforcement skewness.
S102:Vacuum impregnation is carried out to the aluminium oxide ceramics of fibre reinforced using sol-gal process, then dries, burns Knot, and room temperature is cooled to, to prepare Si-Al-C coatings.Specifically, a certain amount of egg is dissolved in a small amount of deionized water first In, and stir to clarify liquid, i.e. liquid A;Produce a certain amount of tetraethyl orthosilicate base silica sol and nitric acid aluminium base aluminum oxide The precursor mixed liquid B of colloidal sol, A is added dropwise in B, that is, obtains C, and is stirred, by the aluminium oxide ceramics of fibre reinforced Vacuum impregnation in liquid C is placed in, is then dried;After drying, the aluminium oxide ceramics of dried fibre reinforced is placed in vacuum Sintering furnace is sintered, after the completion of sintering, keeps vacuum to cool to room temperature with the furnace, and the fibre reinforced oxidation containing antioxidant coating is made Aluminium ceramic composite.Compared with powder sintering method prepares aluminium oxide ceramics, preparing aluminium oxide ceramics using sol-gel process can So that sintering temperature is dropped into 1300 DEG C from 1800 DEG C, equipment requirement and energy resource consumption are greatly reduced.The Si- that the present invention is used Al-C antioxidant coatings are very fine and close, and being well combined for alumina substrate, can effective reinforcing material inoxidizability.
According to a kind of fibre reinforced alumina ceramic composite material of the present invention, including:Reinforcement, matrix and anti-oxidant Coating.Wherein, reinforcement is carbon felt.Carbon fiber is as the reinforcement of aluminium oxide ceramics, and its specific strength and specific modulus be high, without compacted Become, fatigue durability is good, and thermal coefficient of expansion is small, corrosion resistance, and the section wellability of alumina sol and carbon fiber is relatively good, Interface binding power is moderate;Carbon fiber ensure that in the form of carbon felt enhancing phase is evenly distributed, it is to avoid particle enhancing and whisker The problem of strengthening skewness.Matrix is submerged in the space of reinforcement by vacuum impregnation technology, is prepared into reinforcement Composite.Compared with powder sintering method prepares aluminium oxide ceramics, preparing aluminium oxide ceramics using sol-gel process will can burn Junction temperature drops to 1300 DEG C from 1800 DEG C, greatly reduces equipment requirement and energy resource consumption.Antioxidant coating applies for Si-Al-C Layer, antioxidant coating wraps up the composite.Si-Al-C antioxidant coatings are very fine and close, and the combination of alumina substrate is good It is good, can effective reinforcing material inoxidizability.
The present invention is described in detail with reference to specific embodiment.
Embodiment 1
Embodiment 1 is a kind of specific preparation process of fibre reinforced alumina ceramic composite material, and it is with aluminum oxide As matrix, using PAN based carbon felt as reinforcement, there are Si-Al-C antioxidant coatings, including step in detail below in surface:
100g aluminum nitrates are taken, deionized water is added, heating water bath is simultaneously stirred, wherein bath temperature is set as 85 DEG C, continuation Stirring in water bath 30min~40min so that aluminum nitrate is tried one's best hydrolysis.Then add in batches 12.5% ammoniacal liquor, until liquid PH is 3.5~5, while further promotion hydrolysis, makes the property of colloidal sol stable, and adjust the size of micelle.Then evaporate Liquid so that aluminum ions concentration is 6mol/L, viscosity is 6mPaS or so, and this concentration and viscosity are ensureing dipping effect In the case of can as far as possible increase pickling efficiency.Then filter, translucent Alumina gel is made.
Once it is densified:Carbon felt (carbon felt physical dimension is about 4.5mm ╳ 5.5mm ╳ 82mm) after ultrasonic cleaning is placed in Vacuum impregnation 2h in Alumina gel, dries 2h after dipping is complete under 50 DEG C of environment, colloidal sol is become gel, then become xerogel And surface is not ftractureed.Dry and vacuum-sintering in high temperature furnace is put into after finishing, heating rate is 4 DEG C~6 DEG C, and predetermined temperature is 1300 DEG C, it is ensured that xerogel is changed into alpha-aluminium oxide.Reach and 2h is incubated after predetermined temperature so that sintering is complete.Then vacuum is kept Room temperature is cooled to, a densification process is completed.
It is densified repeatedly:The step of to be once densified, as a cycle, is repeated 12 times, complete after 12 densification cycles Into the densification process of composite, it is 2.8g/cm that density, which is made,3Fibre reinforced alumina ceramic composite material.
Prepare Si-Al-C antioxidant coatings:100mL egg is dissolved in a little deionized water, and stirred to clarify Liquid, i.e. liquid A;40mL tetraethyl orthosilicate, 20g aluminum nitrates and 4g hexamethylenetetramines is taken slowly, equably to mix at room temperature In the mixed liquor for dissolving in 60mL deionized waters and 10mL ethanol, and stir, tetraethyl orthosilicate base silica sol and nitric acid is made The first body mixed liquor of aluminium base alumina sol, i.e. liquid B;Liquid in liquid A is added dropwise to liquid B and uniform stirring, liquid C is obtained;Will Fibre reinforced alumina ceramic composite material is placed in liquid C and vacuum impregnation 1h is after 40 DEG C of drying;In lasting vacuumized conditions Under, by dried fibre reinforced alumina ceramic composite material in 1400 DEG C, 30min is sintered, egg is rich in macromolecular Protein, more than 700 DEG C can be carbonized that there is provided a large amount of activated carbon sources.Coating prepare reaction principle be:
2Si2O(s)+2Al2O3(s)+7C(s)→4SiAlC(s)+2CO(g)+CO2(g)
After the completion of sintering, close stove cooling and also keep being evacuated to room temperature, the fibre reinforced oxygen containing antioxidant coating is made Change aluminium composite material.
Embodiment 2
Embodiment 2 is a kind of specific preparation process of fibre reinforced alumina ceramic composite material, and it is with aluminum oxide As matrix, using PAN based carbon felt as reinforcement, there are Si-Al-C antioxidant coatings, including step in detail below in surface:
100g aluminum nitrates are taken, deionized water is added, heating water bath is simultaneously stirred, wherein bath temperature is set as 90 DEG C, continuation Stirring in water bath 30min~40min so that aluminum nitrate is tried one's best hydrolysis.Then in batches add 15% ammoniacal liquor, until liquid PH For 3.5~5, it is further promote hydrolysis while, make the property of colloidal sol stable, and adjust the size of micelle.Then liquid is evaporated Body so that aluminum ions concentration is 5mol/L, viscosity is 6mPaS or so, and this concentration and viscosity are ensureing dipping effect In the case of can as far as possible increase pickling efficiency.Then filter, translucent Alumina gel is made.
Once it is densified:Carbon felt (carbon felt physical dimension is about 4.5mm ╳ 5.5mm ╳ 82mm) after ultrasonic cleaning is placed in Vacuum impregnation 2h in Alumina gel, dries 2h after dipping is complete under 50 DEG C of environment, colloidal sol is become gel, then become xerogel And surface is not ftractureed.Dry and vacuum-sintering in high temperature furnace is put into after finishing, heating rate is 4~6 DEG C, and predetermined temperature is 1400 DEG C, it is ensured that xerogel is changed into alpha-aluminium oxide.Reach and 2h is incubated after predetermined temperature so that sintering is complete.Then vacuum cooled is kept To room temperature, a densification process is completed.
It is densified repeatedly:The step of to be once densified, as a cycle, is repeated 12 times, complete after 12 densification cycles Into the densification process of composite, it is 2.6g/cm that density, which is made,3Fibre reinforced alumina ceramic composite material.
Prepare Si-Al-C antioxidant coatings:100mL egg is dissolved in a little deionized water, and stirred to clarify Liquid, i.e. liquid A;30mL tetraethyl orthosilicate, 18g aluminum nitrates and 4g hexamethylenetetramines is taken slowly, equably to mix at room temperature In the mixed liquor for dissolving in 65mL deionized waters and 15mL ethanol, and stir, tetraethyl orthosilicate base silica sol and nitric acid is made The first body mixed liquor of aluminium base alumina sol, i.e. liquid B;Liquid in liquid A is added dropwise to liquid B and uniform stirring, liquid C is obtained;Will Fibre reinforced alumina ceramic composite material is placed in liquid C and vacuum impregnation 1h is after 35 DEG C of drying;In lasting vacuumized conditions Under, by dried fibre reinforced alumina ceramic composite material in 1200 DEG C, 30min is sintered, egg is rich in macromolecular Protein, more than 700 DEG C can be carbonized that there is provided a large amount of activated carbon sources.Coating prepare reaction principle be:
2Si2O(s)+2Al2O3(s)+7C(s)→4SiAlC(s)+2CO(g)+CO2(g)
After the completion of sintering, close stove cooling and also keep being evacuated to room temperature, the fibre reinforced oxygen containing antioxidant coating is made Change aluminium composite material.
According to the present invention a kind of fibre reinforced alumina ceramic composite material, carbon fiber as aluminium oxide ceramics increasing Qiang Ti, its specific strength and specific modulus are high, and no creep, fatigue durability is good, and thermal coefficient of expansion is small, corrosion resistance, and aluminum oxide is molten The section wellability of glue and carbon fiber is relatively good, and interface binding power is moderate.Carbon fiber ensure that enhancing phase in the form of carbon felt It is evenly distributed, it is to avoid the problem of particle enhancing and whisker reinforcement skewness.By vacuum impregnation technology by fibre reinforced The density domination of alumina ceramic composite material is more than or equal to 2.5g/cm3, considerably increase the mechanical strength of material.With Powder sintering method prepares aluminium oxide ceramics and compared, using sol-gel process prepare aluminium oxide ceramics can by sintering temperature from 1800 DEG C drop to 1300 DEG C, greatly reduce equipment requirement and energy resource consumption.The Si-Al-C antioxidant coatings that the present invention is used are non- Chang Zhimi, and being well combined for alumina substrate, can effective reinforcing material inoxidizability.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show The description of example " or " some examples " etc. means to combine specific features, structure, material or the spy that the embodiment or example are described Point is contained at least one embodiment of the present invention or example.In this manual, to the schematic representation of above-mentioned term not Identical embodiment or example must be directed to.Moreover, specific features, structure, material or the feature of description can be with office Combined in an appropriate manner in one or more embodiments or example.In addition, in the case of not conflicting, the skill of this area Art personnel can be tied the not be the same as Example or the feature of example and non-be the same as Example or example described in this specification Close and combine.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned Embodiment is changed, changed, replacing and modification.

Claims (10)

1. a kind of preparation method of fibre reinforced alumina ceramic composite material, it is characterised in that comprise the following steps:
S101:Using Alumina gel as precursor, vacuum impregnation is carried out to carbon felt, then will be caused with the impregnated carbon felt of Alumina gel Densification process, to prepare the aluminium oxide ceramics of fibre reinforced;
S102:Vacuum impregnation is carried out to the aluminium oxide ceramics of fibre reinforced using sol-gal process, then dries, sinters, and Room temperature is cooled to, to prepare Si-Al-C coatings.
2. a kind of preparation method of fibre reinforced alumina ceramic composite material according to claim 1, its feature exists In in step s 102, the aluminium oxide ceramics progress vacuum impregnation process to fibre reinforced is aoxidized using tetraethyl orthosilicate base The mixed liquor of Ludox, nitric acid aluminium base alumina sol and egg solution composition.
3. a kind of preparation method of fibre reinforced alumina ceramic composite material according to claim 2, its feature exists In in step s 102, the preparation of the mixed liquor comprises the following steps:
Take 30mL~40mL tetraethyl orthosilicate, 15g~25g aluminum nitrate and a certain amount of hexamethylenetetramine add 55mL~ To prepare tetraethyl orthosilicate base silica sol and nitric acid aluminium base alumina sol in 65mL water and alcohol mixeding liquid;
100mL~130mL egg is added into the tetraethyl orthosilicate base silica sol and nitric acid aluminium base alumina sol Clear solution.
4. a kind of preparation method of fibre reinforced alumina ceramic composite material according to claim 1, its feature exists In in step S101, densif iotacation processing step is specially:After the impregnated carbon felt drying of the use Alumina gel, according to 4 DEG C/min~6 DEG C/min heating rate is warming up to 1200 DEG C~1400 DEG C, vacuum-sintering 1h~3h is subsequently cooled to room temperature.
5. a kind of preparation method of fibre reinforced alumina ceramic composite material according to claim 1 or 4, its feature It is, in step S101, the precursor is nitric acid Alumina gel, wherein, aluminum ions concentration is 3mol/L~4mol/L, aluminium The viscosity of colloidal sol is 4mPaS~6mPaS.
6. a kind of preparation method of fibre reinforced alumina ceramic composite material according to claim 1, its feature exists In in step s 102, sintering temperature is 1200 DEG C~1400 DEG C.
7. a kind of preparation method of fibre reinforced alumina ceramic composite material according to claim 6, its feature exists In the preparation method of the nitric acid Alumina gel comprises the following steps:
Excessive aluminum nitrate is added to the water, to prepare aluminum nitrate solution;
The aluminum nitrate solution is heated to 85 DEG C~90 DEG C, after aluminum nitrate is completely dissolved, 10%~15% ammoniacal liquor is added PH value to liquid is 3.5~5.0, and then evaporating moisture makes aluminum ions concentration reach after 5mol/L~6mol/L, filters, takes Filtrate, that is, obtain aluminum nitrate colloidal sol.
8. a kind of fibre reinforced alumina ceramic composite material, it is characterised in that including:
Reinforcement, the reinforcement is carbon felt;
Matrix, described matrix is submerged in by vacuum impregnation technology in the space of the reinforcement, is prepared into the reinforcement Composite;
Antioxidant coating, the antioxidant coating is Si-Al-C coatings, and the antioxidant coating wraps up the composite.
9. a kind of fibre reinforced alumina ceramic composite material as claimed in claim 8, it is characterised in that the carbon fiber The density for strengthening alumina ceramic composite material is more than or equal to 2.5g/cm3
10. a kind of fibre reinforced alumina ceramic composite material as claimed in claim 8, it is characterised in that the carbon felt For PAN based carbon felt.
CN201610391203.7A 2016-06-03 2016-06-03 Carbon fiber reinforced alumina ceramic composite material and preparation method thereof Active CN106966744B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610391203.7A CN106966744B (en) 2016-06-03 2016-06-03 Carbon fiber reinforced alumina ceramic composite material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610391203.7A CN106966744B (en) 2016-06-03 2016-06-03 Carbon fiber reinforced alumina ceramic composite material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN106966744A true CN106966744A (en) 2017-07-21
CN106966744B CN106966744B (en) 2020-04-07

Family

ID=59334737

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610391203.7A Active CN106966744B (en) 2016-06-03 2016-06-03 Carbon fiber reinforced alumina ceramic composite material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN106966744B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108342897A (en) * 2018-02-12 2018-07-31 匡邓吉 A kind of carbon fiber surface aluminium oxide nano film and preparation method thereof
CN108865334A (en) * 2018-06-05 2018-11-23 上海加美实业有限公司 A kind of porcelain fluorine lube oil additive and lubricating oil
CN113185313A (en) * 2021-05-14 2021-07-30 山东工业陶瓷研究设计院有限公司 Carbon fiber reinforced ceramic matrix composite and preparation method thereof
WO2023103209A1 (en) * 2021-12-07 2023-06-15 天津爱思达新材料科技有限公司 Preparation method for modified carbon fiber-toughened alumina self-healing ceramic

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102206089A (en) * 2011-04-07 2011-10-05 中国人民解放军国防科学技术大学 Preparation method for reinforcing mullite by using three-dimensional carbon fiber fabric
CN105367106A (en) * 2015-12-04 2016-03-02 中国人民解放军国防科学技术大学 Carbon-fiber-reinforced zirconium carbide composite material and preparation method therefor
CN105421033A (en) * 2015-11-06 2016-03-23 湖南博望碳陶有限公司 Preparation method of fiber, ceramic and metal three-dimensional network composite material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102206089A (en) * 2011-04-07 2011-10-05 中国人民解放军国防科学技术大学 Preparation method for reinforcing mullite by using three-dimensional carbon fiber fabric
CN105421033A (en) * 2015-11-06 2016-03-23 湖南博望碳陶有限公司 Preparation method of fiber, ceramic and metal three-dimensional network composite material
CN105367106A (en) * 2015-12-04 2016-03-02 中国人民解放军国防科学技术大学 Carbon-fiber-reinforced zirconium carbide composite material and preparation method therefor

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
谢征芳: "用溶胶-凝胶法制备碳纤维三维编织物增强氧化铝基复合材料的研究", 《国防科技大学学报》 *
陈照峰等: "硅溶胶强化辅助制备C纤维增韧氧化铝结合莫来石陶瓷基复合材料", 《航空材料学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108342897A (en) * 2018-02-12 2018-07-31 匡邓吉 A kind of carbon fiber surface aluminium oxide nano film and preparation method thereof
CN108865334A (en) * 2018-06-05 2018-11-23 上海加美实业有限公司 A kind of porcelain fluorine lube oil additive and lubricating oil
CN113185313A (en) * 2021-05-14 2021-07-30 山东工业陶瓷研究设计院有限公司 Carbon fiber reinforced ceramic matrix composite and preparation method thereof
WO2023103209A1 (en) * 2021-12-07 2023-06-15 天津爱思达新材料科技有限公司 Preparation method for modified carbon fiber-toughened alumina self-healing ceramic

Also Published As

Publication number Publication date
CN106966744B (en) 2020-04-07

Similar Documents

Publication Publication Date Title
CN106966744A (en) A kind of fibre reinforced alumina ceramic composite material and preparation method thereof
CN105503227B (en) A kind of preparation method of stereo fabric enhancing silicon carbide diamond composite
CN107032816A (en) A kind of silicon carbide nanometer line enhancing C/C SiC ZrB2The preparation method of ceramic matric composite
CN107805064A (en) A kind of preparation method of fiber reinforced high-temperature-resistant magnesium aluminate spinel aeroge
CN106045550B (en) The preparation method of SiC-ZrC gradient modifying carbon/carbon composite materials
CN103922778A (en) Three-dimensional alumina fiber fabric reinforced oxide ceramic and preparation method thereof
CN109851336A (en) A kind of fine and close continuously mullite nano ceramic fibre and preparation method thereof of high-modulus
CN104926346B (en) A kind of alumina fibre fabric containing interface phase strengthens silicon carbide ceramics and preparation method thereof
CN105780126B (en) A kind of preparation method of the porous mullite formed by generated in-situ whisker overlap joint
CN107445639A (en) A kind of preparation method of carbon/carbon porous body
CN108484194A (en) A kind of Al2O3-SiO2Based composites and its fast preparation method
CN106587901B (en) The preparation method of high temperature resistance and high strength rigidity heat-barrier material
CN102964128B (en) Sol-gel preparation method of Yb2Si2O7 powder
CN109384475A (en) A kind of joint raising SiCfThe method of/SiC ceramic matrix composite material high temperature water resistant oxygen corrosion performance
CN102603344B (en) Preparing process of silicon carbide whisker toughened zirconium diboride ceramic
CN110092650B (en) Light high-strength acicular mullite porous ceramic, preparation method thereof and filter
CN103922794B (en) Three-dimensional aluminum oxide fabric strengthens porous mullite pottery and preparation method thereof
CN104926345B (en) A kind of alumina fibre strengthens carborundum aluminum silicate ceramic and preparation method thereof
CN106090081A (en) A kind of preparation method of composite carbon ceramic material brake disc
CN107640976A (en) Three-dimensional carborundum fiber preform enhancing yttrium silicate composite and preparation method thereof
CN101407420A (en) Method for preparing non-grain boundary phase porous silicon nitride ceramic based on carbon thermal reduction
CN103664218B (en) High-tenacity high-strength far infrared ceramic and preparation method thereof
CN105780120B (en) A kind of Y2Si2O7Whisker and preparation method thereof
CN106187224A (en) A kind of heat-barrier material compositions based on hollow zirconium and preparation method
CN107034379B (en) A kind of preparation method of high-volume fractional oxidation aluminium ceramics enhancing aluminium composite material

Legal Events

Date Code Title Description
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant