CN106904952A - A kind of high-temperature-resistant high alumina fibre enhancing composite and preparation method thereof - Google Patents
A kind of high-temperature-resistant high alumina fibre enhancing composite and preparation method thereof Download PDFInfo
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- CN106904952A CN106904952A CN201710025221.8A CN201710025221A CN106904952A CN 106904952 A CN106904952 A CN 106904952A CN 201710025221 A CN201710025221 A CN 201710025221A CN 106904952 A CN106904952 A CN 106904952A
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Abstract
The present invention relates to a kind of high-temperature-resistant high alumina fibre enhancing composite and preparation method thereof, the present invention is with the continuous alumina fiber precast body of two-dimentional cloth laying, 2.5D braidings or the braiding of orthogonal three-dimensional as reinforcement, matrix is prepared with silica and the compound maceration extract of the well mixed double nano of aluminum oxide, solidified by low temperature precuring in vacuum pressure impregnation, pressure-fired, pressure-fired, atmosphere programs intensification Fractional Heat-treatment the step of, the alumina fibre enhancing composite for finally giving, the mass ratio of silica and aluminum oxide is 19 in composite:1~12:8, the volume content of alumina fibre is 30~60%, resistance to elevated temperatures and mechanical behavior under high temperature that the composite for preparing has, and material density is high, material mechanical properties reach 310 ± 30MPa, 1100 DEG C of stretchings reach 135 ± 20MPa by force, and 1200 DEG C of tensile strengths reach 90 ± 10MPa, and the performance compared to similar quartz fibre enhancing silica oxides/oxide composite improves 4~5 times.
Description
Technical field
The present invention relates to a kind of high-temperature-resistant high alumina fibre enhancing composite and preparation method thereof, belong to ceramic base
Composite field.
Background technology
With the upgrading of the fast-developing and weaponry of China's space flight and aviation cause, material system is proposed gently
The requirements at the higher level that matter, Strengthening and Toughening high, highly reliableization, temperature resistant grade are improved, be with Continuous Fiber Reinforced Ceramic Matrix Composites
The advanced composite material of representative is capable of achieving 30%~50% weight loss effect due to being compared with traditional material, and intensity is quite, can
Good by property, resistance to elevated temperatures is remarkable, therefore suffers from more and more extensive concern.At this stage, advanced composite material has not only turned into
The mainstay material scheme of advanced aircraft design, obtains on bullet, arrow, star, ship and more carrys out sufficient application, in civil aircraft, vapour
Also more and more significant effect has been given play in the fields such as turner industry, nuclear industry.Oxide fibre strengthens oxide ceramics base composite wood
Expect the one kind for advanced composite material, its fiber and matrix are multiple with non-oxidized substance fiber reinforced ceramic-base based on oxide
Condensation material is compared, its problem for not existing high-temperature oxydation, can be worked long hours under high temperature aerobic environment, will not be because of oxidation
And form catastrophic destruction.Therefore under long-time high temperature resistant aerobic environment, oxide fibre enhancing oxide composite
It is an important development direction.Alumina fibre strengthens temperature in use of the composite due to fiber in oxidizing atmosphere and can reach
More than 1400 DEG C, it is expected to be applied at aspects such as turbogenerator, combustion chamber, antenna houses.(F.W.Zok.Developments
In oxide fiber composites.J.Am.Ceram.Soc., 89,3309-3324, (2006), K.A.Keller,
G.Jefferson,and R.J.Kerans.Oxide-oxide composites,in Handbook of Ceramic
Composites,editedby N.A.Bansal(Kluwer Academic,2005),pp.377–421)。
At present in addition to quartz fibre enhancing silica-base composite material, the more oxide fibre enhancing oxidation of research
Thing composite is that alumina fibre strengthens composite.Quartz fibre enhancing silica-base composite material be at present research and
Strengthen oxide composite using oxide fibre the most ripe, it is general to be prepared using sol-gel process, but by
There is crystallization at 1200 DEG C or so in silica, therefore the material is not suitable for making for a long time in 1200 DEG C of high temperature above
With.Alumina fibre composite is to start to have triggered more concern after above-mentioned application bottleneck is highlighted, and aluminum oxide is fine
Dimension composite is mainly with alumina fibre (i.e. principal component be salic fiber) as reinforcing fiber, but it is current for
Composition of continuous alumina fiber enhancing oxide composite and preparation method thereof is showed no detailed report.
The content of the invention
Drawbacks described above it is an object of the invention to overcome prior art, there is provided a kind of high-temperature-resistant high alumina fibre increases
Strong composite, the composite has excellent resistance to elevated temperatures and mechanical behavior under high temperature, and material density is high, comprehensive
Can be good.
Another object of the present invention is to provide a kind of high-temperature-resistant high alumina fibre to strengthen the system of composite
Preparation Method.
What above-mentioned purpose of the invention was mainly achieved by following technical solution：
A kind of high-temperature-resistant high alumina fibre strengthens composite, and the composite is to strengthen with alumina fibre
Body, with silica and the complex phase ceramic matrix of aluminum oxide formation as matrix, wherein the quality of the silica and aluminum oxide
Than being 19:1~12:8, the volume content of the alumina fibre is 30~60%.
In above-mentioned high-temperature-resistant high alumina fibre enhancing composite, the alumina fibre reinforcement is continuous oxygen
Change the integral fabric that aluminum fiber passes through two-dimentional cloth laying, 2.5D or orthogonal three-dimensionals method is sutured or woven.
A kind of high-temperature-resistant high alumina fibre strengthens the preparation method of composite, comprises the following steps：
Step (1), alumina fibre reinforcement is carried out into purification heat treatment；
Step (2), Nano silica sol and nano alumina powder are mixed, disperseed by ball milling or ultrasound, shape
Into compound maceration extract, the viscosity of the compound maceration extract is 30~150mPas；
Step (3), the alumina fibre reinforcement purified after heat treatment is placed in the compound maceration extract and carries out vacuum
And pressure impregnation；
Step (4), the alumina fibre reinforcement that will be impregnated with compound maceration extract carry out precuring below 250 DEG C；
Step (5), the alumina fibre reinforcement after precuring at 800~1200 DEG C is carried out into Fractional Heat-treatment so that
Densification, obtains alumina fibre enhancing composite blank；
Step (6), the alumina fibre is strengthened into composite blank repeat step (three)~step (5), work as oxygen
Change aluminum fiber enhancing composite blank rate of body weight gain≤2wt%, terminate preparation process, obtain final alumina fibre enhancing multiple
Condensation material.
In the preparation method of above-mentioned high-temperature-resistant high alumina fibre enhancing composite, the oxygen in the step (1)
It is that continuous alumina fiber is sutured by two-dimentional cloth laying, 2.5D or orthogonal three-dimensionals method or braiding is formed to change aluminum fiber reinforcement
Integral fabric；The volume content of the alumina fibre reinforcement is 30~60%.
In the preparation method of above-mentioned high-temperature-resistant high alumina fibre enhancing composite, purified in the step (1)
Heat treatment temperature is 380~750 DEG C, and heat treatment time is 0.5~8h.
In the preparation method of above-mentioned high-temperature-resistant high alumina fibre enhancing composite, formed in the step (2)
The specific method of compound maceration extract is as follows：
By nano alumina powder and deionized water with 30:100~1.5:After 100 mass ratio mixing, dispersant is added, obtained
It is 5 according to mass ratio by Nano silica sol and nano alumina powder suspension to nano alumina powder suspension：1~0.2：1
Ratio mixes, and is disperseed using the method for ball milling or ultrasound afterwards, forms compound maceration extract.
In the preparation method of above-mentioned high-temperature-resistant high alumina fibre enhancing composite, in the Nano silica sol
SiO2Solid phase weight/mass percentage composition be 15%~45%, SiO2Size be 10~100nm；The chi of the nano alumina powder
Very little is 50~300nm.
In the preparation method of above-mentioned high-temperature-resistant high alumina fibre enhancing composite, the dispersant is CELUNA
D-305, BYK-154 or BYK-191；The quality of the dispersant is the 0.05~6.0% of nano alumina powder quality.
In the preparation method of above-mentioned high-temperature-resistant high alumina fibre enhancing composite, the rotating speed of the ball milling is
600~1200r/min, Ball-milling Time is 10~200min.
In the preparation method of above-mentioned high-temperature-resistant high alumina fibre enhancing composite, vacuum in the step (3)
Dipping and alternately 1~3 time of pressure impregnation, vacuum-impregnated vacuum is 10~200Pa, dip time is 30~
180min；The pressure that pressure impregnation is used is 0.15~4.5MPa, and dip time is 30~180min.
It is pre- in the step (4) in the preparation method of above-mentioned high-temperature-resistant high alumina fibre enhancing composite
It is solidificated under the pressure-fired of 0.15~0.75MPa and is divided into two stages and carries out, atmosphere is air or nitrogen, first stage precuring
Carried out at a temperature of 110~150 DEG C, soaking time is 1~4h, second stage precuring is carried out at a temperature of 200~250 DEG C,
Soaking time is 1~10h.
In the preparation method of above-mentioned high-temperature-resistant high alumina fibre enhancing composite, it is segmented in the step (5)
Heat treatment is taken temperature programming to be segmented and is carried out, and the condition of specific heat treatment is：Room temperature~800 DEG C, heat-treating atmosphere is air, empty
In 0.05~5L/min, heating rate is 0.05~6 DEG C/min for the flow control of gas, and soaking time is 2~8h；800~target
Maximum temperature, heat-treating atmosphere is nitrogen, and the flow of nitrogen is 0.05~5L/min, and heating rate is 0.05~6 DEG C/min；
Soaking time is 2~8h under target maximum heat treatment temperature.
In the preparation method of above-mentioned high-temperature-resistant high alumina fibre enhancing composite, the target maximum temperature is
1000~1300 DEG C.
The present invention has the advantages that compared with prior art：
(1), material system design of the present invention is that, with alumina fibre as reinforcement, aluminum oxide, silica complex phase ceramic are
Matrix, obtains uniform " double nano is combined maceration extract ", with low temperature in vacuum pressure in the way of chemical modification and physics ball milling
The technique of precuring improves the consistency of material and the retention rate of powder, final to obtain by circulating dipping heat-treating methods
High-temperature oxidation resistant composite with excellent room temperature and mechanical behavior under high temperature, and material density is high, the present invention is by system
The optimization design of standby process condition and technological parameter so that the alumina fibre enhancing composite of preparation has more excellent
Different resistance to elevated temperatures and mechanical behavior under high temperature, more excellent combination property.
(2) the complex phase ceramic shape of silica and aluminum oxide is selected in, material system design of the invention in matrix design
Formula, by adjusting the ratio of silica and aluminum oxide, can be adjusted to the modulus of composite and linear expansion coefficient, carry
Thermal matching between high microsteping and matrix.
(3), the dipping that the present invention is used is " double nano is combined maceration extract ", i.e., with Ludox, nano alumina powder, divide
Powder and deionized water are formulated compound impregnating agent, and nano alumina powder jointed uniform introducing is made by the selection to dispersant
In maceration extract, the solid volume content in maceration extract is improve, improve pickling efficiency；Nano alumina powder has burning higher
Knot activity, also improves alumina component retention rate in the composite, substantially increases the consistency of material；It is single with using
Only Ludox and nano alumina powder separately impregnate or Ludox and micrometer alumina powder dipping, and its pickling efficiency improves 40
~70%, the consistency of material improves 15~38%.
(4), the method for present invention low temperature precuring in cure stage uses pressure-fired, can effectively suppress solidification process
In volumetric expansion and hole formation, greatly improve the consistency of material, with normal pressure solidification mode compared with, the densification of material
Degree improves 10~20%.
(5), the present invention is densified in heat treatment densification stage using air and nitrogen atmosphere Fractional Heat-treatment, Neng Gou
High-temperature area effectively suppresses the creep of fiber, and compared with whole section is heat-treated using air, 1400 DEG C of Tensile strengths are carried
It is high by 20~30%.
(6) the alumina fibre enhancing composite that, prepared by the present invention has excellent resistance to elevated temperatures and high-temperature mechanics
Performance, mechanical properties reach 310 ± 30MPa, and modulus is that 90~150MPa is adjustable, and thermal coefficient of expansion is in (1~5) × 10-6/
K is adjustable, and 1100 DEG C of tensile strength is 135 ± 20MPa, and 1200 DEG C of tensile strength is 90 ± 10MPa, and 1400 DEG C of stretching is strong
It is 70 ± 10MPa to spend, 1500 DEG C of 60 ± 10MPa of tensile strength；Strengthen silica-base composite material compared to quartz fibre,
The mechanical properties of alumina fibre enhancing oxide composite improve 200~350%, 1200 DEG C of tensile strengths and carry
300~400%, 1400 and 1500 DEG C of tensile strengths high have the raising of matter.
Brief description of the drawings
Fig. 1 be the embodiment of the present invention 1 in high-temperature-resistant high alumina fibre enhancing composite room temperature tensile fracture it is microcosmic
Pattern；
Fig. 2 be the embodiment of the present invention 2 in high-temperature-resistant high alumina fibre enhancing 1500 DEG C of stretching fractures of composite it is micro-
See pattern.
Specific embodiment
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings：
High-temperature-resistant high alumina fibre of the present invention strengthens composite with alumina fibre as reinforcement, with silica
It is matrix with the complex phase ceramic matrix that aluminum oxide is formed, wherein the mass ratio of silica and aluminum oxide is 19:1~12:8, oxygen
The volume content for changing aluminum fiber is 30~60%, and the volume content of the complex phase ceramic matrix that silica and aluminum oxide are formed is 70
~40%.Alumina fibre reinforcement is that continuous alumina fiber passes through two-dimentional cloth laying, the suture of 2.5D or orthogonal three-dimensionals method
Or the integral fabric of braiding.Composite is represented by Al2O3f/SiO2-Al2O3。
High-temperature-resistant high alumina fibre of the present invention strengthens the preparation method of composite, specifically includes following steps：
Step (1) is sutured with two-dimentional cloth laying, the method for 2.5D or orthogonal three-dimensionals or the continuous aluminium oxide of braiding is fine
Dimension precast body is reinforcement, and the volume content of fibre reinforcement is 30~60%.
Step (2), the alumina fibre precast body that step (1) is prepared carries out purifying hot place in being put into Ma Fulu
Reason, heat treatment temperature is 380~750 DEG C, and heat treatment time is 0.5~8h.
Step (3), by nano alumina powder and deionized water with 30:100~1.5:After 100 mass ratio mixing, add
0.05~6.0% dispersant, dispersant be CELUNA D-305 (Zhong jing grease Co., Ltd.), BYK-154 (Bi Ke chemistry) or
BYK-191 (Bi Ke chemistry), 10~120min of ultrasound, until uniform dispersion liquid is formed, then by solid phase weight/mass percentage composition
It is 15%~45% Nano silica sol and nano alumina powder suspension according to mass ratio 5:1~0.2:1 ratio mixing, passes through
The method of ball milling or ultrasound is disperseed, and the rotating speed of ball mill is 600~1200r/min, and Ball-milling Time is 10~200min, directly
To viscosity stablization, dispersed " double nano is combined maceration extract " is formed, when the viscosity of maceration extract reaches 30~150mPas side
Can be used.
SiO in Nano silica sol2Solid phase weight/mass percentage composition be 15%~45%, SiO2Size for 10~
100nm；The size of nano alumina powder is 50~300nm.
Step (4), the alumina fibre precast body that step (2) is obtained be placed in that step (3) obtains " double nano is multiple
Close maceration extract " in, the method for circulating dipping by vacuum state and pressure state is impregnated, and vacuum-impregnated vacuum is 10
~200Pa, dip time is 30~180min；The pressure of pressure impregnation be 0.15~4.5MPa, dip time be 30~
180min.Vacuum impregnation and pressure impregnation alternately 1~3 time.
Step (5), the alumina preform that step (4) is obtained is carried out the pressure-fired precuring treatment of maceration extract, Gu
Change process is carried out respectively under the pressure-fired of 0.15~0.75MPa, and atmosphere is air or nitrogen, and the first stage, precuring was 110
Carried out at~150 DEG C, second stage precuring is carried out at a temperature of being solidificated in 200~250 DEG C, two soaking times of temperature section point
Not Wei 1~4h and 1~10h, precuring total time be respectively 2~14h.Pressure-fired in the present invention refers to an atmospheric pressure
1.1~2.0 times of malleation.
Step (6), carry out Fractional Heat-treatment to be densified at 800~1200 DEG C, obtain alumina fibre enhancing composite wood
Material blank, Fractional Heat-treatment is taken temperature programming to be segmented and is carried out, and the maximum temperature for being heat-treated densification is 1000~1300 DEG C, tool
Body heat treatment condition be：Room temperature~800 DEG C heat-treating atmosphere is air, and the flow control of air rises in 0.05~5L/min
Warm speed is 0.05~6 DEG C/min, and soaking time is 2~8h；(1000~1300 DEG C) heat treatment gas of 800~target maximum temperature
Atmosphere is nitrogen, and the flow of nitrogen is 0.05~5L/min, and heating rate is 0.05~6 DEG C/min；Temperature is heat-treated in target highest
Soaking time is 2~8h under degree (i.e. 1000~1300 DEG C).
Step (7), alumina fibre composite blank repeat step (the four)~step (6) 3~10 times that will be obtained,
When alumina fibre composite blank rate of body weight gain≤2wt% (i.e. increased quality with weightening before quality ratio ×
100%), it is considered as densification process to terminate, obtains fine and close alumina fibre enhancing composite.
Material system design of the invention is that, with High-strength aluminum oxide fiber as reinforcement, silica and aluminum oxide are according to one
Fixed ratio forms complex phase ceramic matrix, the wherein mass ratio (m of silica and aluminum oxideSiO2:mAl2O3) 19:1~12:8
Range-controllable.Due to when matrix is made up of silica completely, although the modulus of material can be effectively reduced, but due to it
Thermal coefficient of expansion and reinforcement alumina fibre difference an order of magnitude, when high temperature is experienced, due to thermal coefficient of expansion between the two
Difference produce thermal mismatching, cause that composite is internal at high temperature easily to produce many micro-cracks, so as to cause material at high temperature
The significantly decline of mechanical property.After a certain proportion of aluminum oxide is added in the base, the heat of matrix can be improved first
The coefficient of expansion, substantially reduces the thermal mismatching between fiber and matrix；Secondly, nano alumina powder and Ludox form homogeneous knot
Structure, sintering character more preferably, can effectively improve the density of composite.Using " the compound dipping of double nano in dipping process
Liquid ", and it is aided with the technique of low temperature precuring in vacuum pressure, the consistency of material and the retention rate of powder can be greatly improved,
Material density improves 15~38%.The High-strength aluminum oxide fiber-reinforced composite with excellent high temperature resistance performance can finally be obtained
Material, the mechanical properties of material reach 310 ± 45MPa, and modulus is that 90~150MPa is adjustable, and thermal coefficient of expansion is in (1~5)
×10-6/ K is adjustable, and 1100 DEG C of tensile strength is 135 ± 20MPa, and 1200 DEG C of tensile strength is 90 ± 10MPa, 1400 DEG C
Tensile strength is 70 ± 10MPa, 1500 DEG C of 60 ± 10MPa of tensile strength；Answered compared to quartz fibre enhancing titanium dioxide silicon substrate
Condensation material, the mechanical properties of alumina fibre enhancing oxide composite improve 200~350%, 1200 DEG C of drawings
Stretching intensity and improve 300~400%, 1400 and 1500 DEG C of tensile strengths has the raising of matter.
The present invention is directed to application of the composite under long-time high temperature aerobic environment, using the oxidation of high-strength, antioxidant
Aluminum fiber uses oxide ceramics as reinforcement, matrix, material is had good resistance to elevated temperatures and high temperature antioxygen in itself
Change performance.Due to alumina fibre, modulus is higher in itself, when composite is used as component, it is desirable to be able to which its modulus is entered
Row allotment, therefore the complex phase ceramic form of silica and aluminum oxide is employed in matrix design, wherein silica is adjustable
The modulus of composite is saved, aluminum oxide adjusts the thermal matching between fiber and matrix, and silica and aluminum oxide are according to certain
Ratio formed complex phase ceramic matrix, the wherein mass ratio (m of silica and aluminum oxideSiO2:mAl2O3) 19:1~12:8 models
Enclose controllable, material system is referred to as Al2O3f/SiO2-Al2O3。
Alumina preform of the present invention using two-dimentional cloth laying, the braiding structure of 2.5D or orthogonal three-dimensionals, 2.5D and orthogonal
The precast body of three-dimensional braiding is integral fabric, it is not necessary to do other treatment；Two-dimentional cloth laying alumina fibre precast body, XY is to adopting
The two-dimentional cloth woven with alumina fibre, Z-direction is punctured or sutured using alumina fibre.The volume content of precast body fiber is
30~60%.Precast body first passed through purified treatment before subsequent step is carried out, typically using 380~750 DEG C of warm high at
Reason, heat treatment time is 0.5~8h.
Embodiment 1
(1), as reinforcement, the volume content of fiber is 42% to the continuous alumina fiber precast body with 2.5D；
(2), the alumina fibre precast body that step (1) is prepared is put into Ma Fulu carries out purification heat treatment, heat
Treatment temperature is 700 DEG C, and heat treatment time is 5h；
(3), by nano alumina powder and deionized water with 28:After 100 mass ratio mixing, 3.5% dispersant is added
CELUNA D-305, ultrasonic 100min, form uniform dispersion liquid；Then by nano-silicon that solid phase weight/mass percentage composition is 40%
Colloidal sol and nano alumina powder suspension are according to mass ratio 1：1.5 ratio mixing, is placed in ball mill, and the rotating speed of ball mill is
800r/min, Ball-milling Time is 100min, and the viscosity of maceration extract is 120mPas after being well mixed；
(4) the alumina fibre precast body that step (2) is obtained, is placed in " the compound dipping of double nano that step (3) is obtained
In liquid ", vacuum impregnation 120min, vacuum is 133Pa, then carries out pressure impregnation, and impregnation pressure is 1.25MPa, during dipping
Between be 120min；
(5) alumina preform that step (4) is obtained, is carried out into first stage precuring, solidification pressure at 130 DEG C first
Power is 0.70MPa, and atmosphere is air, and pre-cure time is 3.5h；Second stage precuring is then carried out at 240 DEG C, is solidified
Pressure is 0.70MPa, and atmosphere is air, and hardening time is 6h.
(6) the alumina fibre precast body that step (5) is obtained, is carried out into temperature programming under air and nitrogen atmosphere, is divided
Section heat treatment.Room temperature~800 DEG C heat-treating atmosphere is air, the flow control of air in 2.5L/min, heating rate is 5 DEG C/
Min, soaking time is 4h, and 800~1200 DEG C of heat-treating atmospheres are nitrogen, and the flow of nitrogen is 2.5L/min, and heating rate is 5
DEG C/min, soaking time is 3h at 1200 DEG C；
(7), repeat step (3)~(6) totally 6 times, rate of body weight gain≤2wt%, densification process terminates, and obtains final oxidation
Aluminum fiber strengthens ceramic matric composite, i.e. Al2O3f/SiO2-Al2O3。
The performance of the present embodiment alumina fibre enhancing ceramic matric composite is as follows：
The density of composite is 2.61g/cm3, mechanical properties are 282MPa, and modulus is 130MPa, 1200 DEG C of drawings
Intensity is stretched for 94MPa, and 1400 DEG C of tensile strengths are 70MPa, and 1500 DEG C of tensile strengths are respectively 61MPa.
As shown in Figure 1 in the embodiment of the present invention 1 high-temperature-resistant high alumina fibre enhancing composite room temperature tensile break
Mouth microscopic appearance, Fig. 2 show high-temperature-resistant high alumina fibre enhancing 1500 DEG C of stretchings of composite in the embodiment of the present invention 2
Fracture micro-appearance, composite is fine and close as seen from the figure, and after experience room temperature tensile properties experiment, fracture is presented obvious fiber
Phenomenon is extracted, ductile rupture pattern is shown as；After 1500 DEG C of high temperature tensile properties experiments of experience, fracture still shows necessarily
Spike protein gene effect, this is that the material possesses the evidence of good mechanical behavior under high temperature.
Embodiment 2
(1), as reinforcement, the volume content of fiber is 38% to the continuous alumina fiber precast body with two-dimentional cloth laying；
(2), the alumina fibre precast body that step (1) is prepared is put into Ma Fulu carries out purification heat treatment, heat
Treatment temperature is 400 DEG C, and heat treatment time is 3h；
(3), by nano alumina powder and deionized water with 15：After 100 mass ratio mixing, 2.0% dispersant is added
CELUNA D-305, ultrasonic 60min, form uniform dispersion liquid；Then by nano-silicon that solid phase weight/mass percentage composition is 40%
Colloidal sol and nano alumina powder suspension are according to mass ratio 1：1 ratio mixing, is placed in ball mill, and the rotating speed of ball mill is
600r/min, Ball-milling Time is 60min, and the viscosity of maceration extract is 50mPas after being well mixed；
(4) the alumina fibre precast body that step (2) is obtained, is placed in " the compound dipping of double nano that step (3) is obtained
In liquid ", vacuum impregnation 1h, vacuum is 100Pa, then carries out pressure impregnation, and impregnation pressure is 0.2MPa, and dip time is
1h；
(5) alumina preform that step (4) is obtained, is carried out into precuring, first stage precuring at 110 DEG C first
Pressure is 0.5MPa, and atmosphere is air, and pre-cure time is 2h, and second stage precuring, solidification pressure are then carried out at 200 DEG C
Power is 0.2MPa, and atmosphere is air, and hardening time is 4h.
(6) the alumina fibre precast body that step (5) is obtained, is carried out into temperature programming under air and nitrogen atmosphere, is divided
Section heat treatment.Room temperature~800 DEG C heat-treating atmosphere is air, the flow control of air in 1.5L/min, heating rate is 2 DEG C/
Min, soaking time is 2h；800~1000 DEG C of heat-treating atmospheres are nitrogen, and the flow of nitrogen is 2L/min, and heating rate is 2
℃/min；Soaking time is 3h at 1000 DEG C；
(7), repeat step (3)~(6) totally 6 times, rate of body weight gain≤2wt%, densification process terminates, and obtains final oxidation
Aluminum fiber strengthens ceramic matric composite, i.e. Al2O3f/SiO2-Al2O3。
The performance of the present embodiment alumina fibre enhancing ceramic matric composite is as follows：
The density of composite is 2.26g/cm3, mechanical properties are 267MPa, and modulus is 115MPa, thermal expansion system
Number is 3.7 × 10-6/ K, 1200 DEG C of tensile strengths are 84MPa, and 1400 DEG C of tensile strengths are 62MPa, 1500 DEG C of tensile strength difference
It is 54MPa.
The above, optimal specific embodiment only of the invention, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
Should all be included within the scope of the present invention.
The content not being described in detail in description of the invention belongs to the known technology of professional and technical personnel in the field.
Claims (13)
1. a kind of high-temperature-resistant high alumina fibre strengthens composite, it is characterised in that：The composite is fine with aluminum oxide
It is reinforcement to tie up, with silica and the complex phase ceramic matrix of aluminum oxide formation as matrix, wherein the silica and oxidation
The mass ratio of aluminium is 19:1~12:8, the volume content of the alumina fibre is 30~60%.
2. a kind of high-temperature-resistant high alumina fibre according to claim 1 strengthens composite, it is characterised in that：It is described
Alumina fibre reinforcement is continuous alumina fiber by two-dimentional cloth laying, the suture of 2.5D or orthogonal three-dimensionals method or braiding
Into integral fabric.
3. a kind of high-temperature-resistant high alumina fibre strengthens the preparation method of composite, it is characterised in that：Comprise the following steps：
Step (1), alumina fibre reinforcement is carried out into purification heat treatment；
Step (2), Nano silica sol and nano alumina powder are mixed, disperseed by ball milling or ultrasound, formed multiple
Maceration extract is closed, the viscosity of the compound maceration extract is 30~150mPas；
Step (3), the alumina fibre reinforcement purified after heat treatment is placed in the compound maceration extract and carries out vacuum and pressure
Power impregnates；
Step (4), the alumina fibre reinforcement that will be impregnated with compound maceration extract carry out precuring below 250 DEG C；
Step (5), the alumina fibre reinforcement after precuring is carried out Fractional Heat-treatment at 800~1200 DEG C to be densified,
Obtain alumina fibre enhancing composite blank；
Step (6), the alumina fibre is strengthened into composite blank repeat step (three)~step (5), work as aluminum oxide
Fibre reinforced composites blank rate of body weight gain≤2wt%, terminates preparation process, obtains final alumina fibre enhancing composite wood
Material.
4. a kind of high-temperature-resistant high alumina fibre according to claim 3 strengthens the preparation method of composite, and it is special
Levy and be：Alumina fibre reinforcement in the step (1) for continuous alumina fiber pass through two-dimentional cloth laying, 2.5D or
Orthogonal three-dimensional method suture or the integral fabric of braiding；The volume content of the alumina fibre reinforcement be 30~
60%.
5. a kind of high-temperature-resistant high alumina fibre according to claim 3 strengthens the preparation method of composite, and it is special
Levy and be：It is 380~750 DEG C that heat treatment temperature is purified in the step (1), and heat treatment time is 0.5~8h.
6. a kind of high-temperature-resistant high alumina fibre according to claim 3 strengthens the preparation method of composite, and it is special
Levy and be：The specific method that compound maceration extract is formed in the step (2) is as follows：
By nano alumina powder and deionized water with 30:100~1.5:After 100 mass ratio mixing, dispersant is added, received
Rice alumina powder suspension, is 5 according to mass ratio by Nano silica sol and nano alumina powder suspension：1~0.2：1 ratio
Mixing, is disperseed using the method for ball milling or ultrasound afterwards, forms compound maceration extract.
7. a kind of high-temperature-resistant high alumina fibre according to claim 6 strengthens the preparation method of composite, and it is special
Levy and be：SiO in the Nano silica sol2Solid phase weight/mass percentage composition be 15%~45%, SiO2Size for 10~
100nm；The size of the nano alumina powder is 50~300nm.
8. a kind of high-temperature-resistant high alumina fibre according to claim 6 strengthens the preparation method of composite, and it is special
Levy and be：The dispersant is CELUNA D-305, BYK-154 or BYK-191；The quality of the dispersant is nano aluminium oxide
The 0.05~6.0% of silty amount.
9. a kind of high-temperature-resistant high alumina fibre according to claim 6 strengthens the preparation method of composite, and it is special
Levy and be：The rotating speed of the ball milling is 600~1200r/min, and Ball-milling Time is 10~200min.
10. a kind of high-temperature-resistant high alumina fibre according to claim 3 strengthens the preparation method of composite, and it is special
Levy and be：Alternately 1~3 time of vacuum impregnation and pressure impregnation in the step (3), vacuum-impregnated vacuum is 10
~200Pa, dip time is 30~180min；The pressure that pressure impregnation is used is 0.15~4.5MPa, dip time is 30~
180min。
A kind of 11. high-temperature-resistant high alumina fibres according to claim 3 strengthen the preparation method of composite, and it is special
Levy and be：Precuring in the step (4) is divided into two stages under the pressure-fired of 0.15~0.75MPa to be carried out, and atmosphere is
Air or nitrogen, first stage precuring are carried out at a temperature of 110~150 DEG C, and soaking time is 1~4h, and second stage is pre- solid
Change is carried out at a temperature of 200~250 DEG C, and soaking time is 1~10h.
A kind of 12. high-temperature-resistant high alumina fibres according to claim 3 strengthen the preparation method of composite, and it is special
Levy and be：Fractional Heat-treatment is taken temperature programming to be segmented and is carried out in the step (5), and the condition of specific heat treatment is：Room temperature~
800 DEG C, heat-treating atmosphere is air, and in 0.05~5L/min, heating rate is 0.05~6 DEG C/min for the flow control of air,
Soaking time is 2~8h；800~target maximum temperature, heat-treating atmosphere is nitrogen, and the flow of nitrogen is 0.05~5L/min,
Heating rate is 0.05~6 DEG C/min；Soaking time is 2~8h under target maximum heat treatment temperature.
A kind of 13. high-temperature-resistant high alumina fibres according to claim 12 strengthen the preparation method of composite, its
It is characterised by：The target maximum temperature is 1000~1300 DEG C.
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| CN116384163B (en) * | 2023-06-05 | 2023-09-05 | 中国航发四川燃气涡轮研究院 | Design method of ceramic matrix composite complex component for aero-engine |
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