CN1718560A - Carbon-fiber reinforced silicon carbide composite material antioxidation coating layer and its preparation method - Google Patents
Carbon-fiber reinforced silicon carbide composite material antioxidation coating layer and its preparation method Download PDFInfo
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- CN1718560A CN1718560A CN 200510031774 CN200510031774A CN1718560A CN 1718560 A CN1718560 A CN 1718560A CN 200510031774 CN200510031774 CN 200510031774 CN 200510031774 A CN200510031774 A CN 200510031774A CN 1718560 A CN1718560 A CN 1718560A
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Abstract
An antioxidizing coated layer of carbon fibre reinforced SiC material is composed of adhesive layer, self-healing layer and impact and corrosion resistant layer. It is prepared through isothermal chemical vapor deposition (CVD) for preparing adhesive layer, coating sludge and sintering for preparing self-healing layer, and isothermal CVD for preparing the impact and corrosion resistant layer.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, be specifically related to a kind of carbon-fiber reinforced silicon carbide composite material antioxidation coating layer and preparation method thereof.
Background technology
The Cf/SiC matrix material has caused concern widely as the elevated temperature heat structured material in the application of Aeronautics and Astronautics and energy field, in the research of developed country's a new generation's engine and hot machine, it is to improve engine or hot machine chamber temperature, and then improves one of the most desirable thermal structure material of energy transformation efficiency.
The Cf/SiC matrix material has good high-temperature mechanical property and thermal characteristics, in inert environments, surpass 2000 ℃ and still can keep mechanical property such as intensity not reduce, have good fracture toughness property and wear resisting property, low thermal coefficient of expansion, high heat conductance, high gasification temperature and good thermal shock resistance.But in oxidizing atmosphere, being higher than 400 ℃ of carbon fibers will oxidation, thereby causes material property to reduce material failure.This is to influence the Cf/SiC matrix material in the medium-term and long-term deadly defect of using of oxidizing atmosphere, must solve the oxidation-resistance problem of Cf/SiC matrix material for this reason.
The raising of the oxidation-resistance of Cf/SiC matrix material can be taked dual mode:
(1) comes the antioxidant property of strongthener by processing to body material.As by in the matrix hole, infiltrating Cr
3Si, MoSi
2, phosphoric acid salt waits and strengthens antioxidant property, perhaps by crossing BN, B on the carbon fiber top layer
4The rete of compounds such as C comes the strongthener antioxidant property, or the like.
(2) antioxidant property by whole oxidation resistant coating strongthener.
But antioxidant property generally by whole oxidation resistant coating strongthener; because the thermal mismatching of coating and matrix can crack; effective protection temperature range of coating is narrower; coating poor effect under the low temperature then when high temperature is effective, when low temperature is effective then often high temperature do not protect effect.
Summary of the invention
Technical problem to be solved by this invention is: at the above-mentioned defective of prior art existence, a kind of oxidation weight loss speed that can reduce the Cf/SiC matrix material is provided, satisfies the Cf/SiC matrix material at Cf/SiC composite material antioxidation coating layer of the medium-term and long-term requirement of using of high temperature oxidation stability environment and preparation method thereof.
The technical scheme that solution the technology of the present invention problem is adopted is: a kind of whole inoxidzable coating of carbon fibre reinforced silicon carbide composite material; it is characterized in that this inoxidzable coating is positioned at outside the carbon fibre reinforced silicon carbide composite material member of required protection; described inoxidzable coating is a three-decker; comprise SiC adhesive linkage, self-healing layer and SiC erosion resistance layer, and putting in order from the inside to the outside is SiC adhesive linkage, self-healing layer and SiC erosion resistance layer successively.
The preparation method of the whole inoxidzable coating of carbon fibre reinforced silicon carbide composite material is characterized in that comprising the steps:
A, employing isothermal chemical vapor deposition method prepare the SiC adhesive linkage;
B, employing mud coating sintering legal system are equipped with the self-healing layer;
C, employing isothermal chemical vapor deposition method prepare SiC erosion resistance layer.
The method that described isothermal chemical vapor deposition method prepares the SiC adhesive linkage is as follows: member is rinsed well, and the oven dry back places chemical vapor deposition stove with the carbon fiber bondage, is precursor with the trichloromethyl silane, H
2Be carrier gas and catalysts, Ar is dilution and shielding gas, and depositing temperature is 900-1300 ℃, and furnace pressure is controlled at below the 10KPa, and depositing time obtained the carbon fibre reinforced silicon carbide composite material member that the surface has adhesive linkage after 10～20 hours.
The preparation method of described self-healing layer is as follows: the self-healing layer is after energy oxidation generation glass state material, sintering aid, organic adhesion agent and solvent are prepared into slurry down by high temperature; be coated on the surface of material members, by after the infrared radiation drying in high temperature inert atmosphere protection stove sintering form.
The material that described high temperature down can oxidation generates vitreous state is that norbide, molybdenum disilicide, sintering aid are yttrium oxide, organic adhesion agent is a polyvinyl alcohol, be followed successively by 2～3: 2～3 by weight: 1: 2～3, at first norbide, molybdenum disilicide, yttrium oxide ball milling are mixed, add polyvinyl alcohol and suitable quantity of water and stir into slurry.
The agglomerating method of described self-healing layer is as follows: will place normal pressure inert atmosphere protection sintering oven by dried sample under infrared radiation; temperature rise rate by 0.5～2 ℃/min is warming up to 100～1100 ℃; be incubated 0.5～2 hour, the taking-up of cooling back obtains coating and contains self-healing layer sample uniformly.
The preparation method of described SiC erosion resistance layer is as follows: the carbon fiber/enhancing composite material of silicon carbide member that will contain even self-healing layer places chemical vapor deposition stove, is precursor with the trichloromethyl silane, H
2Be carrier gas and catalysts, Ar is dilution and shielding gas, and depositing temperature is 900-1300 ℃, and furnace pressure is controlled at below the 10KPa, and depositing time 10～20 hours promptly obtains SiC erosion resistance layer.
The beneficial effect that the present invention produced is:
The present invention improves the anti-oxidation protection effect of coating by adopting the self-healing layer that can produce the self-healing effect in than large-temperature range; can reduce the oxidation weight loss speed of Cf/SiC matrix material; make the Cf/SiC composite element in bigger temperature range, have good antioxidant property, satisfy the Cf/SiC matrix material in the medium-term and long-term requirement of using of high temperature oxidation stability environment.
Description of drawings
Fig. 1 is a Cf/SiC composite material antioxidation coating layer structural representation of the present invention;
Fig. 2 is that the XRD figure spectrum of CVD-SiC and PIP-SiC compares;
Fig. 3 is a CVD-SiC coating crack Photomicrograph;
Fig. 4 is the synoptic diagram of oxygen by the diffusion of coating crack;
Fig. 5 is the SEM photo of three layers of coating section;
Fig. 6 is no anti-oxidation protection coating sample oxidation weight loss curve;
Fig. 7 is an individual layer SiC coating sample oxidation weight loss curve;
Fig. 8 is the low-temperature oxidation weight-loss curve of three layers of coating protection sample;
Fig. 9 is three layers of coating protection sample high temperature oxidation weight-loss curve;
Among the figure: 1-SiC erosion resistance layer, 2-self-healing layer, 3-SiC adhesive linkage, 4-member.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing.
The basic function of oxidation resistant coating is that body material and outside oxidizing atmosphere are isolated, and realize its isolation features effectively, and the oxidation resistant coating system must satisfy some basic demands:
1), coated material is stable in the protection temperature range, coating system and body material have good bonding effect, do not peel off between coating and matrix and coating and the coating or separate;
2), close thermal expansivity (CTE) is arranged between coated material and matrix;
3), coated material has the low oxygen and the spread coefficient of carbon;
4), good chemistry and mechanical compatibility are arranged between coated material and matrix;
5), use the erosion can be subjected to hot-fluid usually as structure unit, use in this environment, coated material must have good anti-erosion property or the like.
The Cf/SiC matrix material usually in hot environment as structure unit, its envrionment temperature may in the very short time, rangeability reach thousands of degrees centigrade.Under so violent temperature disturbance, thermal expansivity between coated material and body material can not mate fully, the thermal expansivity of body material is lower, when temperature is lower than the preparation temperature of coating, coating can form tiny crack, and these tiny cracks will form the passage that oxygen is diffused into material internal.In order effectively to protect, prolong the anti-oxidant life-span, coating system must have self-healing function, can form flowable glassy phase, fills up tiny crack, and barrier oxidation atmosphere is by these crackle diffusions.
As Fig. 1; Fig. 1 is a Cf/SiC composite material antioxidation coating layer structural representation of the present invention; this inoxidzable coating is positioned at outside the Cf/SiC composite element 4 of required protection; described inoxidzable coating is a three-decker; comprise SiC adhesive linkage 3, self-healing layer 2 and SiC erosion resistance layer 1, and putting in order from the inside to the outside is SiC adhesive linkage 3, self-healing layer 2 and SiC erosion resistance layer 1 successively.
SiC coating by the chemical vapor deposition method preparation is very fine and close, the diffusion and the infiltration of energy barrier gas.The stoichiometric ratio of Si and C is 1: 1, and good high-temperature antioxidant property and chemical stability are arranged.Thermal expansivity is lower, and high high-temp stability is good.Therefore adopt the adhesive linkage of SiC, both utilized the advantage of SiC coating self, also meet Cf/SiC performance of composites feature as Cf/SiC matrix material oxidation resistant coating system.
Fig. 2 is that the XRD figure spectrum of CVD-SiC and PIP-SiC compares, the result as can be known thus, the SiC matrix of PCS cracking preparation has similar crystalline structure to CVD-SiC, PIP-SiC is again rich carbon simultaneously, therefore PIP-SiC can be coated with interlayer with CVD-SiC at carbon fiber and plays transition layer, so to adopt the CVD-SiC coating be the most rational selection as the adhesive linkage of coating system.
Because the member body material is different with the thermal expansivity that is coated with interlayer, along with variation of temperature, can the generation thermal mismatching between coating and matrix, cause coating shedding or crack.The SiC of body material is Polycarbosilane (PCS) cracking preparation, and rich carbon is also incomplete same with the SiC chemical constitution by the CVD prepared; Simultaneously, body material contains the enhancing body carbon fiber of about 40% volume fraction, though Polycarbosilane (PCS) cracked SiC and CVD-SiC coating are by close forming and similar structure, can play a transition role, make the CVD-SiC coating bonding effect preferably be arranged with body material, but when the preparation that is lower than the CVD-SiC coating when envrionment temperature acquired a certain degree, coating still can crack.Fig. 3 is the stereoscan photograph of CVD-SiC coating crack, and the width that can see crackle is several microns.
If all regard coating and matrix as elastomerics, the generation of crackle will overcome YIELD STRENGTH.The generation temperature T c of crackle can calculate by following formula:
E is the Young's modulus of coated material in the formula, σ
RUBe the yield strength of coated material, α
cAnd α
mBe respectively the linear expansivity of coating and body material, TF is the preparation temperature of coating, and the preparation temperature of isothermal CVD-SiC coating is exactly a depositing temperature, and it is also low more that the crackle of the low more then coating of preparation temperature produces temperature.When T＜Tc, coating cracks, and oxygen spreads by crackle.
Fig. 3 is the Photomicrograph of the CVD-SiC coating crack pattern of Cf/SiC matrix material under the room temperature.
When crackle generated, the crackle width of CVD-SiC coating was shown below with variation of temperature:
E(T)＝E0(1-TE/TF)
E0 is the crackle width under the room temperature, and TE is the temperature of coating, and TF is the coating preparation temperature.Along with the crackle width of the rising coating of temperature reduces.When temperature reached the preparation temperature of coating, the crackle width became 0.
When there was crackle in coating, oxygen can arrive material internal swimmingly by crackle, carbon oxide fiber and matrix (shown in Figure 4).
Oxidation resistant coating of the present invention is made up of three layers of coating, and the centre has the self-healing layer 2 of self-healing function by the CB that can form glass state material after the oxidation
4, MoSi
2Deng composition, therefore in oxidative environment oxidized after, at high temperature these flowable vitreous state products can enter in the crackle of coating, the healing coating crack, what stop oxygen passes through to play the anti-oxidation protection effect.
Adhesive linkage and erosion resistance layer are made up of CVD-SiC.Adhesive linkage and erosion resistance layer adopt isothermal chemical vapor deposition method (CVD) preparation by CVD-SiC among the present invention.Compare with other technology, chemical vapor deposition method prepares the SiC coating and has the following advantages:
(1) technological temperature is low, can obtain crystal form SiC coating about 1000 ℃;
(2) very high density and purity, crystal structure directional property are good; Preparation process condition is to be precursor with trichloromethyl silane (MTS), H
2Be carrier gas and catalysts, Ar is dilution and shielding gas, and depositing temperature is 900-1300 ℃, and furnace pressure is controlled at below the 10KPa, depositing time 10～20 hours.
Self-healing active function layer can oxidation generate glass state material CB down by high temperature
4, MoSi
2Deng compound powder and Y
2O
3, ZrO
2Form Deng sintering aid; add after an amount of organic adhesion agent and solvent be prepared into slurry; be coated on the surface of material members, by after the infrared radiation drying in high temperature inert atmosphere protection stove sintering form (1100～1500 ℃ of firing temperatures), Fig. 5 is the SEM photo of three layers of coating section
The present invention has tested the oxidation weight loss speed of Cf/SiC composite element, and to containing three layers of coating system sample respectively in oxidation was tested sample after (12day) in 288 hours in still air under the differing temps flexural strength.Test result shows, three layers of coating system in still air under the constant temperature to material to good anti-oxidation protection effect, the sample in 500 ℃ and 800 ℃ of-1300 ℃ of temperature ranges after the long-time oxidation is still protected flexural strength preferably.
Fig. 6 is no anti-oxidation protection coating sample oxidation weight loss curve; Show that thus sample is not having under the situation of coating protection as easy as rolling off a log oxidizedly, no matter high temperature or low-temperature oxidation weight loss rate are all very fast, and accelerates with temperature rising rate of oxidation.Weight-loss curve shows under 600 ℃ that sample weight descends rapidly in 6 hours, reaches balancing segment.800 ℃ of-1200 ℃ of temperature next in 3 hours oxidation weight loss rapidly, reach balancing segment.Fig. 7 is an individual layer SiC coating sample oxidation weight loss curve, because the protection of SiC coating is arranged, antioxidant property is better than no coating sample far away.
Compare with the sample of individual layer CVD-SiC coating protection with no coating protection sample, the sample of three layers of coating protection then has good antioxidant property.Oxidation weight loss speed is slowed down 1-2 the order of magnitude.But the anti-oxidation protection effect of three layers of coating obviously shows as and is better than 600 ℃ and 700 ℃ more than 800 ℃, and oxidative mass loss is low main because material is difficult for oxidation at this under this temperature in the time of 500 ℃.Fig. 8 is the low-temperature oxidation weight-loss curve of three layers of coating protection sample, oxidation 288h weightlessness about 7% in the time of 500 ℃, and the oxidative mass loss when 600 ℃ and 700 ℃ is then bigger, and the oxidative mass loss of 288h is respectively 21.9% and 33.3%.Fig. 9 is three layers of coating protection sample high temperature oxidation weight-loss curve, and the rate of weight loss behind 900 ℃, 1000 ℃ and the 1100 ℃ of oxidation 288h shows 900 ℃ of-1100 ℃ of temperature range undercoat to have fabulous anti-oxidation protection effect all below 3%.800 ℃, 1200 ℃ and 1300 ℃ of oxidative mass loss are than 900 ℃, 1000 ℃ and 1100 ℃ big, but still remain on lower level, and the maximum rate of weight loss of oxidation 288h does not surpass 7%.From the oxidation weight loss test-results, three layers of coating system that the present invention is made up of CVD-SiC adhesive linkage, self-healing active function layer, CVD-SiC anti-impact erosion layer have good anti-oxidation protection effect at 800 ℃-1300 ℃.
Table 1 is three layers of coating sample through after the long-time oxidation of 288h, the weight retention rate of sample and flexural strength test result.In 500 ℃ and 800 ℃ of-1300 ℃ of temperature ranges, the oxidative mass loss of sample is lower, and minimum only is 2.3%, and is maximum also less than 7%, and flexural strength remains on more than the 252.3MPa, and that maximum is 452.9MPa.
The weight retention rate and the flexural strength of three layers of coating sample of table 1
| Oxidizing temperature/ | 500 | 600 | 700 | 800 | 900 | 1000 | 1100 | 1200 | 1300 |
| Weight retention rate/% | 92.9 | 78.1 | 66.7 | 96.8 | 98.3 | 97.7 | 97.5 | 95.2 | 93.6 |
| Flexural strength/MPa | 358.5 | 89.3 | 372.8 | 443.1 | 452.9 | 397.9 | 352.0 | 252.3 |
Embodiment 1:
The preparation of step 1:SiC adhesive linkage: will be by the Cf/SiC composite element (50mm * 5mm * 4mm) rinse well of polymeric preceramic body Polycarbosilane (PCS) impregnating cracking technology preparation, the oven dry back places chemical vapor deposition stove with the carbon fiber bondage, chemical vapor deposition stove is warming up to 900 ℃, feeds H behind the constant temperature
2, with H
2(MTS) brings in the chemical vapor deposition stove with trichloromethyl silane, feeds Ar as dilution and shielding gas, H
2Flow velocity keeps 500ml/min, and the Ar flow velocity keeps 500ml/min, vacuumizes to keep furnace pressure to be controlled at being 600Pa-800Pa, and depositing time 20 hours is prepared the SiC adhesive linkage.
Step 2: the preparation of self-healing layer: take by weighing CB
4, MoSi
2Each 30 gram, Y
2O
3Micro mist 10 gram mixes being placed in the ball milling cylinder ball milling 2 hours.Behind the ball milling mixed powder is mixed with 30 gram polyvinyl alcohol, add an amount of water and make slurry.With slurry coating in the Cf/SiC composite element surface that prepares the SiC adhesive linkage; dry under infrared lamp irradiation; burning till of self-healing layer: will under infrared radiation, place normal pressure inert atmosphere protection sintering oven by dried sample; temperature rise rate by 1 ℃/min is warming up to 1100 ℃, insulation 30min.The taking-up of cooling back obtains coating and contains self-healing layer sample uniformly.
The preparation of step 3:SiC erosion resistance layer: the Cf/SiC composite element that will contain even self-healing layer places chemical vapor deposition stove, and chemical vapor deposition stove is warming up to 900 ℃, feeds H behind the constant temperature
2, with H
2(MTS) brings in the chemical vapor deposition stove with trichloromethyl silane, feeds Ar as dilution and shielding gas.H
2Flow velocity keeps 200ml/min, and the Ar flow velocity keeps 150ml/min, vacuumizes to keep furnace pressure to be controlled at being 200Pa-300Pa, and depositing time 15 hours obtains containing the sample of three layers of coating.
Embodiment 2:
The preparation of step 1:SiC adhesive linkage: chemical vapor deposition stove is warming up to 1300 ℃, feeds H behind the constant temperature
2, with H
2(MTS) brings in the chemical vapor deposition stove with trichloromethyl silane, feeds Ar as dilution and shielding gas.H
2Flow velocity keeps 800ml/min, and the Ar flow velocity keeps 400ml/min, vacuumizes to keep furnace pressure to be controlled at being 900Pa-1000Pa.Depositing time 10 hours.
Embodiment 3:
Step 2: take by weighing CB
4, MoSi
2Each 20 gram, Y
2O
3Micro mist 10 gram mixes being placed in the ball milling cylinder ball milling 2 hours.Behind the ball milling mixed powder is mixed with 20 gram polyvinyl alcohol, add an amount of water and make slurry.With slurry coating in the Cf/SiC composite element surface that prepares the SiC adhesive linkage; dry under infrared lamp irradiation; burning till of self-healing layer: will under infrared radiation, place normal pressure inert atmosphere protection sintering oven by dried sample; temperature rise rate by 1 ℃/min is warming up to 1500 ℃; insulation 30min, the taking-up of cooling back obtains coating and contains self-healing layer sample uniformly.
Claims (8)
1, a kind of whole inoxidzable coating of carbon fibre reinforced silicon carbide composite material; it is characterized in that this inoxidzable coating is positioned at outside the carbon fibre reinforced silicon carbide composite material member of required protection; described inoxidzable coating is a three-decker; comprise SiC adhesive linkage, self-healing layer and SiC erosion resistance layer, and putting in order from the inside to the outside is SiC adhesive linkage, self-healing layer and SiC erosion resistance layer successively.
2, the preparation method of the whole inoxidzable coating of a kind of carbon fibre reinforced silicon carbide composite material as claimed in claim 1 is characterized in that comprising the steps:
A, employing isothermal chemical vapor deposition method prepare the SiC adhesive linkage;
B, employing mud coating sintering legal system are equipped with the self-healing layer;
C, employing isothermal chemical vapor deposition method prepare SiC erosion resistance layer.
3, the preparation method of the whole inoxidzable coating of carbon fibre reinforced silicon carbide composite material according to claim 2, it is characterized in that the method that described isothermal chemical vapor deposition method prepares the SiC adhesive linkage is as follows: member is rinsed well, the oven dry back places chemical vapor deposition stove with the carbon fiber bondage, with the trichloromethyl silane is precursor, H
2Be carrier gas and catalysts, Ar is dilution and shielding gas, and depositing temperature is 900-1300 ℃, and furnace pressure is controlled at below the 10KPa, and depositing time obtained the carbon fibre reinforced silicon carbide composite material member that the surface has adhesive linkage after 10～20 hours.
4, the preparation method of the whole inoxidzable coating of carbon fibre reinforced silicon carbide composite material according to claim 3; the preparation method who it is characterized in that described self-healing layer is as follows: the self-healing layer is after energy oxidation generation glass state material, sintering aid, organic adhesion agent and solvent are prepared into slurry down by high temperature; be coated on the surface of material members, by after the infrared radiation drying in high temperature inert atmosphere protection stove sintering form.
5, according to the preparation method of the whole inoxidzable coating of the described carbon fibre reinforced silicon carbide composite material of right claim 4, the material that it is characterized in that under the described high temperature can oxidation generating vitreous state is that norbide, molybdenum disilicide, sintering aid are yttrium oxide, organic adhesion agent is a polyvinyl alcohol, be followed successively by 2～3: 2～3 by weight: 1: 2～3, at first norbide, molybdenum disilicide, yttrium oxide ball milling are mixed, add the polyethylene alcohol and water and stir into slurry.
6, according to the preparation method of claim 4 or the whole inoxidzable coatings of 5 described carbon fibre reinforced silicon carbide composite materials; the agglomerating method that it is characterized in that described self-healing layer is as follows: will place normal pressure inert atmosphere protection sintering oven by dried sample under infrared radiation; temperature rise rate by 0.5～2 ℃/min is warming up to 100～1100 ℃; be incubated 0.5～2 hour, the taking-up of cooling back obtains coating and contains self-healing layer sample uniformly.
7, according to the preparation method of the whole inoxidzable coating of any described carbon fibre reinforced silicon carbide composite material in the claim 3,4,5, the preparation method who it is characterized in that described SiC erosion resistance layer is as follows: the carbon fiber/enhancing composite material of silicon carbide member that will contain even self-healing layer places chemical vapor deposition stove, with the trichloromethyl silane is precursor, H
2Be carrier gas and catalysts, Ar is dilution and shielding gas, and depositing temperature is 900-1300 ℃, and furnace pressure is controlled at below the 10KPa, and depositing time 10～20 hours promptly obtains SiC erosion resistance layer.
8, the preparation method of the whole inoxidzable coating of carbon fibre reinforced silicon carbide composite material according to claim 6, the preparation method who it is characterized in that described SiC erosion resistance layer is as follows: the carbon fiber/enhancing composite material of silicon carbide member that will contain even self-healing layer places chemical vapor deposition stove, with the trichloromethyl silane is precursor, H
2Be carrier gas and catalysts, Ar is dilution and shielding gas, and depositing temperature is 900-1300 ℃, and furnace pressure is controlled at below the 10KPa, and depositing time 10～20 hours promptly obtains SiC erosion resistance layer.
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