CN105967755A - Mullite whisker toughened mullite oxidation-resistant coating for carbon/carbon composite material as well as preparation method thereof - Google Patents
Mullite whisker toughened mullite oxidation-resistant coating for carbon/carbon composite material as well as preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating 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
- C04B41/5076—Coating 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 with masses bonded by inorganic cements
- C04B41/5089—Silica sols, alkyl, ammonium or alkali metal silicate cements
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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Abstract
The invention discloses a mullite whisker toughened mullite oxidation-resistant coating for a carbon/carbon composite material as well as a preparation method thereof, and belongs to the field of preparation technology of oxidation-resistant coatings. A molten salt method and an in situ reaction method are combined in order to prepare the mullite whisker toughened mullite composite oxidation-resistant external coating for the carbon/carbon composite material. Firstly, a simple molten salt method is used for preparing a mullite whisker buffer layer, so that on one hand wetability between an internal coating and an external coating is improved, and on the other hand bonding strength between the internal coating and the external coating is improved; secondly, the in situ reaction method is selected, in order to produce a silicate external coating with good oxidation resistant performance, low oxygen permeability, and high temperature resistance in situ. The external coating is prepared in a high temperature oxidation atmosphere, so that cost is reduced, and a new path is initiated. Components of the coating can be easily controlled, in order to prepare a plurality of silicate coatings for adapting to needs of coatings of different temperature sections. The method has the advantages of short preparation period, simple process, low cost, and wide application prospects.
Description
Technical field
The invention belongs to ORC preparing technical field, relate to one prepare carbon/carbon compound material be combined
The method of external coating, is specifically related to a kind of carbon/carbon composite mullite crystal whisker toughened mullite antioxidation and is coated with
Layer and preparation method thereof.
Background technology
C/C composite is otherwise known as carbon fiber carbon based composites, owing to it is by single carbon group
Become, not only there is the ablation resistance that charcoal and graphite material are excellent, the advantages such as low-density, thermal coefficient of expansion are low,
And under high temperature, also have excellent mechanical property.The property that especially its intensity goes up not down with the increase of temperature
Can so that it is become one of the most rising hi tech and new material, be widely used as aerospace technology
The ablator in field and thermal structure material.But, C/C composite is in the temperature oxidation more than 500 DEG C
Rapid oxidation under atmosphere, which greatly limits its application, and therefore the oxidation protection problem of C/C composite becomes
For one of study hotspot in recent years.It is carried out high-temperature oxidation resistant protection the application of its high temperature is had simultaneously
Important meaning.
ORC is considered as the effective ways solving carbon/carbon compound material oxidant protection under high temperature problem.
For preventing C/C composite from high temperature aoxidizing, domestic and international research worker has carried out substantial amounts of theory and test
Research, develops multiple ORC system.
At present, the coating system developed has glass, metal, pottery and composite coating.Glass coating is permissible
The crackle that produces due to deformation when material for repairing is on active service, but Conventional glass mobility at high temperature and volatilization
Property limits its use under higher temperature and air-flow Scouring Condition.Precious metal alloys coating such as Ir-Al-Si
Etc. being demonstrated by preferable non-oxidizability, but its cost is high and oxidation protection is limited in one's ability.Ceramic coating is current
The focus of research, and commonly used be silicon based ceramic.Its key problem in technology is to utilize SiO under high temperature2Or it is anti-
The SiO that should generate2Fill the defects such as crackle in coating, as the infiltration sealing material and stopping oxygen.
What research was more at present is silicon based ceramic coating.In order to combine the advantage of various material, researcher also developed
Composite coating with SiC as transition zone, such as SiC/MoSi2[J.F.Huang,B.Wang,H.J.Li,M.Liu,
L.Y.Cao,C.Y.Yao.A MoSi2/SiC oxidation protective coating for carbon/carbon
composites,Corros.Sci.53(2011)834-839.]、SiC/Mullite[K.T.Wang,L.Y.Cao,
J.F.Huang,J.Fei,A mullite/SiC oxidation protective coating for carbon/carbon
composites,J.Eur.Ceram.Soc.33(2013)191-198.]、SiC/Yttrium silicate[M.
Huang,K.Z.Li,H.J.Li,J.F.Huang,,Yttrium silicate coatings for SiC coated C/C
composites prepared by atmospheric plasma spraying,Carbon.48(2010)
3974-3977.] by numerous studies, find that above-mentioned ceramic coating has a common shortcoming, that is, due to
The fragility that ceramic material is intrinsic, it is easy to crack during thermal shock, even comes off.Due to silica-based pottery
The SiO that porcelain autoxidation produces2Amount is few, and high temperature and under washing away airflow function volatilization serious, it is difficult to healing
Big crackle.The most usually need to prepare one layer of glassy layer again on surface and carry out packing crackle.But glassy layer is at height
Speed ion stream washes away also the most quickly volatilization under environment, reduces packing effect.
At the antioxygenic property of full warm area and crackle extension in the coating is slowed down, research in order to improve coating
Person develops with nanowire-toughened composite coating, SiC nanowire toughness reinforcing SiC-Si coating [Y.H.Chu, H.J.
Li,L.Li,L.H.Qi,Oxidation protection of C/C composites by ultra long SiC
Nanowire-reinforced SiC-Si coating, Corros.Sci.84 (2014) 204 208.], SiC nanowire
Toughness reinforcing MoSi2-SiC-Si coating [Fu Qian-Gang, Li He-Jun, Li Ke-Zhi, Shi Xiao-Hong, Hu
Zhi-Biao,Huang Min,SiC whisker-toughened MoSi2-SiC-Si coating to protect
Carbon/carbon composites against oxidation, Carbon.2006,44,1866.] etc..Answering of preparation
Close coating and C/C composite can be played effective protective action.But in order to make ORC towards longevity
The directions such as life, high temperature resistant, antiscour are developed also to be needed to be continually striving to.Mullite (thermal coefficient of expansion is 5.0 ×
10-6/ DEG C) ceramic material refractoriness height, good thermal shock, chemical resistance of concrete, creep resistant, loading softening temperature
Degree is high, volume stability is preferable high grade refractory well, is widely used in each field.Mullite crystal whisker
Have high temperature resistant, wear-resistant, antioxidation, thermal coefficient of expansion are less, elevated temperature strength is relatively big, thermal shock resistance
Preferably and there is the excellent properties such as high-temerature creep is little, and with mullite crystal whisker plasticizing mullite avoid due to
The mismatch of thermal coefficient of expansion and crack.Therefore, become raising with mullite crystal whisker enhancing mullite not come
Feldspar toughness and the effective way of reliability.And up to the present, with its grinding as ORC
Study carefully the most rarely found report.
Up to the present the preparation method of external coating is varied, mainly has following several: supercritical fluid
Technology, chemical gaseous phase deposits, investment, formed in situ, sol-gel process, molten slurry coating reaction, quick-fried
Fried spraying and ultrasonic spray method etc..Above-mentioned preparation technology exists that the production cycle is long, complex process, is coated with
The layer problem poor with matrix binding ability, and the preparation of coating completes the most under the high temperature conditions, preparation process
High to equipment requirements, preparation cost is high.
At present, use molten-salt growth method to combine in-situ method and prepare mullite crystal whisker plasticizing mullite antioxidation external coating
Method have not been reported.
Summary of the invention
For the defect overcoming above-mentioned prior art to exist, it is an object of the invention to provide a kind of carbon/carbon multiple
Condensation material mullite crystal whisker plasticizing mullite ORC and preparation method thereof, the method is simple to operate, right
Equipment requirements is low, and reaction time is short, low cost, uses the method can prepare thickness uniform, and structure causes
Close carbon/carbon composite mullite crystal whisker toughened mullite ORC.
The present invention is to be achieved through the following technical solutions:
The invention discloses the system of a kind of carbon/carbon composite mullite crystal whisker toughened mullite ORC
Preparation Method, comprises the following steps:
1) Al is pressed2(SO4)3·18H2O:Na2SO4The mass ratio of=9:10, takes Al2(SO4)3·18H2O and
Na2SO4, fully after mixing, prepare mixing double salt A；
2) SiC-C/C composite sample (with the C/C composite sample of SiC coating) is carried out
Ultrasonic cleaning, after drying, by SiC-C/C composite sample: mixing double salt A=(1～3): the matter of 19
Amount ratio, is embedded in SiC-C/C composite sample in mixing double salt A, at 900～950 DEG C, at heat
After reason, cooling；
3) will be through step 2) process after sample boiling water clean, until clean unreacted fused salt, then
By samples dried, prepare the sample (mullite/SiC-C/C) with mullite crystal whisker layer；
4) by Si powder and Al2O3The mixed powder of powder composition is scattered in what Ludox and distilled water mixed
In mixed solution, prepare the slip B1 that mixed powder concentration is 200～300g/L, by ultrasonic for slip B1 shake
After swinging, then through magnetic agitation, prepare slip B2；
5) slip B2 is uniformly painted on step 3) prepare the specimen surface with mullite crystal whisker layer,
Dry at room temperature, repeat brushing, dry operation 5～10 times after, dry；
6) by step 5) dry the sample that obtains under argon shield, at 1500 DEG C, it is incubated 2～4h,
Prepare carbon/carbon composite mullite crystal whisker toughened mullite ORC.
Step 1) described in abundant mixing, be by Al2(SO4)3·18H2O and Na2SO4It is placed in mortar,
It is fully ground 30～60min.
Step 2) it is SiC-C/C composite sample to be placed in ultrasonic cleaning in ethanol, then in 50～80 DEG C
Lower drying.
Step 2) it is that mixing double salt A is placed in corundum crucible, SiC-C/C composite sample is embedded
In mixing double salt A, then corundum crucible is placed in Muffle furnace, heat treatment 30～60min.
Step 3) it is that clean sample is dried in the electric drying oven with forced convection of 60～90 DEG C 1～3h.
Step 4) in, in the mixed solution that Ludox and distilled water mix, Ludox and distilled water
Volume ratio is 1:3；In mixed powder, Si powder and Al2O3The mol ratio of powder is 2:3.
Step 4) in by slip B1 ultrasonic vibration 10～20min, then on magnetic stirring apparatus stir 1～3h,
Obtain slip B2.
Step 5) described in drying be at 50～80 DEG C, be dried 1～2h.
Step 6) it is that sample drying obtained carries out isothermal holding in high-temperature atmosphere furnace.
The invention also discloses the carbon/carbon composite mullite using said method to prepare crystal whisker toughened not come
Stone ORC, this ORC thickness is uniform, compact structure, surface flawless, coating and matrix
Bond strength is big.
Compared with prior art, the present invention has a following useful technique effect:
The inventive method well combines the advantage of both mullite and mullite crystal whisker, uses molten-salt growth method knot
Close in-situ reaction to be prepared for outside carbon/carbon composite mullite crystal whisker toughened mullite compound anti-oxidation being coated with
Layer, first, with simple process for preparing mullite crystal whisker by molten salt cushion, on the one hand can improve inside and outside coating
Between wettability, on the other hand improve the inside and outside bond strength with layer；Secondly, select in-situ reaction,
In-situ preparation antioxygenic property is good, oxygen permeability is low, resistant to elevated temperatures silicate external coating.The present invention uses
High temperature oxidative atmosphere prepares external coating, the most cost-effective, has also started a new road.This method
Easily the component of coating is controlled, multiple silicate coating can be prepared, adapt to different temperatures section coating
Need.The inventive method manufacturing cycle is short, technical process simple, low cost, has broad application prospects.
Through the carbon/carbon composite mullite crystal whisker toughened mullite ORC that the inventive method prepares,
Thickness is uniform, compact structure, and without obvious hole and crackle, inside and outside coating is tightly combined, the most significantly
Boundary.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of mullite crystal whisker layer prepared under the conditions of embodiment 3；
Fig. 2 is the SEM photograph of mullite crystal whisker layer prepared under the conditions of embodiment 3；Wherein, (a) not
Carry out the surface SEM photograph of stone crystal whisker layer；B () is the section SEM photograph of mullite crystal whisker layer；
Fig. 3 is the XRD figure spectrum of mullite crystal whisker plasticizing mullite coating prepared under the conditions of embodiment 3；
Fig. 4 is the SEM photograph of mullite crystal whisker plasticizing mullite coating prepared under the conditions of embodiment 3；
Wherein, (a) is surface SEM photograph；B () is section SEM photograph.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, described in the present invention
Explain rather than limit.
Embodiment 1
A kind of preparation method of carbon/carbon composite mullite crystal whisker toughened mullite ORC, including
Following steps:
(1) analytically pure Al is weighed respectively for the ratio of 9:10 in mass ratio2(SO4)3·18H2O and Na2SO4
In mortar, it is fully ground 60min to mix homogeneously, obtains the mixing double salt A of the two.
(2) the C/C composite sample (SiC-C/C) with SiC coating is placed in ethanol surpasses
Sound cleans, and then takes out sample and dries at 80 DEG C, weighs SiC-C/C sample mass, with mass ratio is
The ratio of 2:19 weighs above-mentioned double salt A in corundum crucible, and is embedded in double salt by SiC-C/C sample.
(3) crucible having embedded SiC-C/C sample is placed in Muffle furnace in 925 DEG C of reaction 40min.
(4) the complete furnace cooling of question response is to after room temperature, takes out；The boiling water of 100 DEG C is washed,
Until cleaning unreacted fused salt, then sample being dried in the electric drying oven with forced convection of 80 DEG C 2h and obtains
Sample (mullite/SiC-C/C) with mullite crystal whisker layer.
(5) by Si powder that mol ratio is 2:3 and nanometer Al2O3The mixed powder of powder composition is scattered in 20mL
The mixed solution that distilled water and the Ludox ratio with volume ratio as 3:1 combine is configured to mixed powder
Concentration is the slip B1 of 200g/L, by slip B1 ultrasonic vibration 10min, then on magnetic stirring apparatus
Stirring 1h, obtains slip B2.
(6) with paintbrush, the slip B2 of (5) gained is painted on equably by (4) gained
Mullite/SiC-C/C specimen surface, and dry at room temperature, put into after being repeated 10 times in baking oven in 50 DEG C
Under be dried 2h.
(7) sample of (6) gained is put in high-temperature atmosphere furnace, protects at 1500 DEG C under argon shield
Temperature 2h, obtains carbon/carbon composite mullite crystal whisker toughened mullite ORC.
Embodiment 2
A kind of preparation method of carbon/carbon composite mullite crystal whisker toughened mullite ORC, including
Following steps:
(1) analytically pure Al is weighed respectively for the ratio of 9:10 in mass ratio2(SO4)3·18H2O and Na2SO4
In mortar, it is fully ground 50min to mix homogeneously, obtains the mixing double salt A of the two.
(2) the C/C composite sample (SiC-C/C) with SiC coating is placed in ethanol surpasses
Sound cleans, and then takes out sample and dries at 70 DEG C, weighs SiC-C/C sample mass, with mass ratio is
The ratio of 3:19 weighs above-mentioned double salt A in corundum crucible, and is embedded in double salt by SiC-C/C sample.
(3) crucible having embedded SiC-C/C sample is placed in Muffle furnace in 950 DEG C of reaction 30min.
(4) the complete furnace cooling of question response is to after room temperature, takes out；The boiling water of 100 DEG C is washed,
Until cleaning unreacted fused salt, then sample being dried in the electric drying oven with forced convection of 90 DEG C 1h and obtains
Sample (mullite/SiC-C/C) with mullite crystal whisker layer.
(5) by Si powder that mol ratio is 2:3 and nanometer Al2O3The mixed powder of powder composition is scattered in 30mL
The mixed solution that distilled water and the Ludox ratio with volume ratio as 3:1 combine is configured to mixed powder
Concentration is the slip B1 of 250g/L, by slip B1 ultrasonic vibration 15min, then on magnetic stirring apparatus
Stirring 2h, obtains slip B2.
(6) with paintbrush, the slip B2 of (5) gained is painted on equably by (4) gained
Mullite/SiC-C/C specimen surface, and drying at room temperature, puts in baking oven at 60 DEG C after being repeated 8 times
It is dried 2h.
(7) sample of (6) gained is put in high-temperature atmosphere furnace, protects at 1500 DEG C under argon shield
Temperature 3h, obtains carbon/carbon composite mullite crystal whisker toughened mullite ORC.
Embodiment 3
A kind of preparation method of carbon/carbon composite mullite crystal whisker toughened mullite ORC, including
Following steps:
(1) analytically pure Al is weighed respectively for the ratio of 9:10 the most in mass ratio2(SO4)3·18H2O and
Na2SO4In mortar, it is fully ground 30min to mix homogeneously, obtains the mixing double salt A of the two.
(2) the C/C composite sample (SiC-C/C) with SiC coating is placed in ethanol surpasses
Sound cleans, and then takes out sample and dries at 60 DEG C, weighs SiC-C/C sample mass, with mass ratio is
The ratio of 1:19 weighs above-mentioned double salt A in corundum crucible, and is embedded in double salt by SiC-C/C sample.
(3) crucible having embedded SiC-C/C sample is placed in Muffle furnace in 900 DEG C of reaction 60min.
(4) the complete furnace cooling of question response is to after room temperature, takes out；The boiling water of 100 DEG C is washed,
Until cleaning unreacted fused salt, then sample being dried in the electric drying oven with forced convection of 60 DEG C 3h and obtains
Sample (mullite/SiC-C/C) with mullite crystal whisker layer.
(5) by Si powder that mol ratio is 2:3 and nanometer Al2O3The mixed powder of powder composition is scattered in 40mL
The mixed solution that distilled water and the Ludox ratio with volume ratio as 3:1 combine is configured to mixed powder
Concentration is the slip B1 of 300g/L, by slip B1 ultrasonic vibration 20min, then on magnetic stirring apparatus
Stirring 3h, obtains slip B2.
(6) with paintbrush, the slip B2 of (5) gained is painted on equably by (4) gained
Mullite/SiC-C/C specimen surface, and drying at room temperature, puts in baking oven at 80 DEG C after being repeated 5 times
It is dried 1h.
(7) sample of (6) gained is put in high-temperature atmosphere furnace, protects at 1500 DEG C under argon shield
Temperature 4h, obtains carbon/carbon composite mullite crystal whisker toughened mullite ORC.
See Fig. 1, the XRD figure spectrum of mullite crystal whisker layer prepared by employing molten-salt growth method, as can be seen from Figure
Molten-salt growth method is used can successfully to prepare mullite crystal whisker layer on SiC-C/C surface.The diffraction peak intensity of mullite is bright
Aobvious less than SiC, this illustrates that the molten-salt growth method corrosion when preparing mullite crystal whisker layer to SiC-C/C is the most little,
Preferable modifying function can be played.
See Fig. 2, be the SEM photograph of prepared mullite crystal whisker layer, can be seen that from Fig. 2 (a),
Prepared mullite crystal whisker layer is formed by collecting pencil whisker uniformly.From the section SEM photograph of Fig. 2 (b)
Can be seen that, by molten-salt growth method SiC-C/C specimen surface prepare uniformly thickness be 10～20 μm not
Carry out stone crystal whisker layer.
See Fig. 3, be the XRD figure spectrum of prepared mullite crystal whisker plasticizing mullite coating, from figure
Can be seen that, this molten-salt growth method combines reaction in-situ can successfully prepare mullite crystal whisker plasticizing mullite coating.
Based on mullite crystalline phase in coating, there is a small amount of unreacted Si and SiO2, this antioxidation to coating
Performance impact is little, in antioxidation process, can gradually form glassy state, thus institute in healing coating in time
The defect existed.
See Fig. 4, be to use molten-salt growth method to combine the mullite crystal whisker plasticizing mullite coating prepared by full-boiled process
SEM photograph.Can be seen that from Fig. 4 (a), prepared carbon/carbon composite mullite is crystal whisker toughened not to be come
Stone ORC surface compact is uniform, without obvious hole and crackle.Can be seen that from Fig. 4 (b), institute
The carbon/carbon composite mullite crystal whisker toughened mullite ORC very dense uniform of preparation, due to
Being prepared for mullite crystal whisker cushion, inside and outside coating is tightly combined, and does not has obvious boundary.
In sum, the present invention uses molten-salt growth method to combine in-situ method to prepare mullite crystal whisker plasticizing mullite antioxygen
Outside the pale of civilization coating, has a following three points advantage:
(1) synthesis temperature can be reduced significantly and shorten the response time, being attributed to the melt due to salt
Being formed, make reacted constituent mobility in the liquid phase strengthen, diffusion rate significantly improves.Simultaneously because fused salt
Being applied between the granule of generation, stop between granule is interconnected, therefore, and the material that molten-salt growth method prepares
Soilless sticking, or the most weakly agglomerated；
(2) shape and size of material can more easily be controlled；
(3), in the course of reaction of molten-salt growth method and cleaning process subsequently, it is also beneficial to the elimination of impurity,
Form high-purity product.The ultimate principle of reaction in-situ is by mixing elemental silicon and good with its moistening
Metal-oxide, being coated on previously prepared has the internally coated specimen surface of SiC, sinters under atmosphere protection
It is pre-formed Si and the metal oxide precursor coating of densification, then in certain temperature and oxidizing atmosphere
Lower pre-oxidation a period of time, then can good with in-situ preparation antioxygenic property, oxygen permeability is low, resistant to elevated temperatures
Silicate external coating.Being unique in that of the method courageously uses high temperature oxidative atmosphere to prepare external coating, no
The most cost-effective, also start a new road.The component of coating is easily controlled by this method,
Multiple silicate coating can be prepared, adapt to different temperatures section coating needs.
Claims (10)
1. a preparation method for carbon/carbon composite mullite crystal whisker toughened mullite ORC, its
It is characterised by, comprises the following steps:
1) Al is pressed2(SO4)3·18H2O:Na2SO4The mass ratio of=9:10, takes Al2(SO4)3·18H2O and
Na2SO4, fully after mixing, prepare mixing double salt A；
2) SiC-C/C composite sample is carried out ultrasonic cleaning, after drying, by SiC-C/C composite wood
Material samples: mixing double salt A=(1～3): the mass ratio of 19, is embedded in SiC-C/C composite sample
In mixing double salt A, at 900～950 DEG C, after heat treatment, cooling；
3) will be through step 2) process after sample boiling water clean, until clean unreacted fused salt, then
By samples dried, prepare the sample with mullite crystal whisker layer；
4) by Si powder and Al2O3The mixed powder of powder composition is scattered in what Ludox and distilled water mixed
In mixed solution, prepare the slip B1 that mixed powder concentration is 200～300g/L, by ultrasonic for slip B1 shake
After swinging, then through magnetic agitation, prepare slip B2；
5) slip B2 is uniformly painted on step 3) prepare the specimen surface with mullite crystal whisker layer,
Dry at room temperature, repeat brushing, dry operation 5～10 times after, dry；
6) by step 5) dry the sample that obtains under argon shield, at 1500 DEG C, it is incubated 2～4h,
Prepare carbon/carbon composite mullite crystal whisker toughened mullite ORC.
Carbon/carbon composite mullite the most according to claim 1 crystal whisker toughened mullite antioxidation is coated with
The preparation method of layer, it is characterised in that step 1) described in abundant mixing, be by Al2(SO4)3·18H2O
And Na2SO4It is placed in mortar, is fully ground 30～60min.
Carbon/carbon composite mullite the most according to claim 1 crystal whisker toughened mullite antioxidation is coated with
The preparation method of layer, it is characterised in that step 2) it is that SiC-C/C composite sample is placed in ethanol
Ultrasonic cleaning, then dries at 50～80 DEG C.
Carbon/carbon composite mullite the most according to claim 1 crystal whisker toughened mullite antioxidation is coated with
The preparation method of layer, it is characterised in that step 2) it is that mixing double salt A is placed in corundum crucible, will
SiC-C/C composite sample is embedded in mixing double salt A, is then placed in Muffle furnace by corundum crucible,
Heat treatment 30～60min.
Carbon/carbon composite mullite the most according to claim 1 crystal whisker toughened mullite antioxidation is coated with
The preparation method of layer, it is characterised in that step 3) it is the electric heating air blast of 60～90 DEG C by clean sample
Drying baker is dried 1～3h.
Carbon/carbon composite mullite the most according to claim 1 crystal whisker toughened mullite antioxidation is coated with
The preparation method of layer, it is characterised in that step 4) in, the mixing that Ludox and distilled water mix is molten
In liquid, Ludox is 1:3 with the volume ratio of distilled water；In mixed powder, Si powder and Al2O3Powder mole
Ratio is 2:3.
Carbon/carbon composite mullite the most according to claim 1 crystal whisker toughened mullite antioxidation is coated with
Layer preparation method, it is characterised in that step 4) in by slip B1 ultrasonic vibration 10～20min, then
Magnetic stirring apparatus stirs 1～3h, obtains slip B2.
Carbon/carbon composite mullite the most according to claim 1 crystal whisker toughened mullite antioxidation is coated with
Layer preparation method, it is characterised in that step 5) described in drying be at 50～80 DEG C, be dried 1～2h.
Carbon/carbon composite mullite the most according to claim 1 crystal whisker toughened mullite antioxidation is coated with
The preparation method of layer, it is characterised in that step 6) it is that sample drying obtained enters in high-temperature atmosphere furnace
Row isothermal holding.
10. the carbon/carbon compound material using in claim 1～9 method described in any one to prepare does not comes
Stone crystal whisker plasticizing mullite ORC, it is characterised in that this ORC thickness is uniform, structure causes
Close, surface flawless, coating is big with substrate combinating strength.
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| CN109942317A (en) * | 2019-04-25 | 2019-06-28 | 西北工业大学 | Surface of carbon/carbon composite mullite crystal whisker-mullite/yttrium aluminosilicate compound anti-oxidation coating and preparation method |
| CN112321331A (en) * | 2020-11-18 | 2021-02-05 | 江西信达航科新材料科技有限公司 | High-temperature-resistant antioxidant composite coating and preparation process thereof |
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| CN104130013A (en) * | 2014-07-10 | 2014-11-05 | 陕西科技大学 | Carbon/carbon composite material SiC whisker toughened mullite composite coating preparation method |
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| CN1793017A (en) * | 2005-11-22 | 2006-06-28 | 武汉理工大学 | Mullite whisker-mullite composite coating and preparation process thereof |
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| CN109942317A (en) * | 2019-04-25 | 2019-06-28 | 西北工业大学 | Surface of carbon/carbon composite mullite crystal whisker-mullite/yttrium aluminosilicate compound anti-oxidation coating and preparation method |
| CN112321331A (en) * | 2020-11-18 | 2021-02-05 | 江西信达航科新材料科技有限公司 | High-temperature-resistant antioxidant composite coating and preparation process thereof |
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