CN105175028A - High-temperature-resistant and thermal-shock-resistant SiC/B4C composite coating and preparation method thereof - Google Patents
High-temperature-resistant and thermal-shock-resistant SiC/B4C composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-temperature-resistant and thermal-shock-resistant SiC/B4C composite coating and a preparation method thereof. The composite coating comprises a SiC coating deposited on a substrate material and a B4C coating deposited on the outer surface of the SiC coating. The SiC and B4C coatings are combined, so that the defects that SiO2 produced by a single-layer SiC coating through oxidation has poor volatility at the low temperature and cannot completely seal cracks of the coating are overcome; meanwhile, B2O3 produced by the B4C through oxidation at the low temperature has good liquidity and effectively blocks invasion of oxygen, when the oxygen invades an inner SiC layer from the outside, the surface temperature of the material is increased, and the SiO2 has the good fluidity, so that the cracks can be sealed effectively.
Description
Technical field
The present invention relates to a kind of high temperature resistant anti-thermal shock SiC/B
4c compound coating and preparation method thereof, belongs to chemical vapour deposition field.
Background technology
Continuous Fiber Reinforced Ceramic Matrix Composites has low density, good mechanical property, thermostability and the excellent specific property such as chemical stability and radiation hardness, in recent years, along with the development of science and technology, more and more extensive in field application such as aerospace, new forms of energy, communications and transportation, and in material surface seal coat, the effects such as good heat insulation, high temperature resistant, anticorrosive, antiscour can be played, at present, the common method preparing coating has plasma spraying, reaction sintering, magnetron sputtering plating, chemical vapour deposition etc.
Plasma spraying.Its ultimate principle adopts the plasma current of direct-current drive as thermal source, stupalith is heated to melting or semi-melting state, and to spray to the method forming the top coat of adhere firmly through pretreated ceramic material surfaces at a high speed, but the method can produce violent noise, high light radiation, obnoxious flavour, metallic dust etc. in spraying process, and small size pores internal surface is difficult to spraying.
Reaction sintering.Its ultimate principle the material of required sintering and binding agent is mixed into liquid state be coated in material surface in advance, then dry, sinter molding under high temperature afterwards, the standby coat-thickness of this legal system generally can reach hundreds of micron, sometimes even several centimetres, but due to the impact of gravity, coating finally often forms uneven thickness and form.
Magnetron sputtering plating.Its ultimate principle utilizes high-octane lotus energy particle to attack target, and the atom of target material surface or molecule are overflowed and deposition process on substrate surface.Sputtering equipment needed for this method is complicated, and need vacuum system and high-tension unit, sedimentation velocity is slow.
In addition, current material surface thermal protection coating such as has single SiC coating, single B
4c coating etc.Only have for single SiC coating for outer surface, due to SiO at low temperatures
2poor fluidity, the finiteness of closed material surface crack is not good enough, and for C/SiC matrix material, due to the difference of thermal expansivity between material and coating, in conjunction with weak between coating and matrix, makes material surface often occur crackle, and for single B
4c coating, higher than under 1200 DEG C of conditions, the B that coating oxidation generates
2o
3become gaseous state, easily volatilization causes oxygen directly contact fiber and make material failure.
Summary of the invention
For the problems referred to above, the object of this invention is to provide a kind of high temperature resistant anti-thermal shock SiC/B
4c compound coating and preparation method thereof.
On the one hand, the invention provides a kind of high temperature resistant anti-thermal shock SiC/B
4c compound coating, described compound coating comprises: be deposited on the SiC coating on base material and the B being deposited on SiC coating outer surface
4c coating.
The present invention is by SiC/B
4c two kinds of phase coatings combine, and effectively overcome the SiO that individual layer SiC coating oxidation generates
2under low temperature, volatility is poor, packing coating itself cannot there is the shortcoming of crackle completely, simultaneously B
4the lower B generated of oxidation under C low temperature
2o
3there is good mobility, effectively block the invasion of oxygen, when oxygen intrudes into SiC internal layer from outward, because now material surface temperature raises, SiO
2there is good fluidity, can effective packing crackle.
And, SiC and B
4between C coating, thermal expansivity is suitable, thermal expansion mismatch between two kinds of coatings will be eased greatly, combination between two kinds of coatings will be tightr, when coating of the present invention is such as used for SiC/SiC matrix material, the difference of thermal expansion coefficients of SiC/SiC matrix material and matrix surface is little, combines closely between coating and matrix.
In addition, SiC and B
4c has higher thermostability, as outmost coating, and B
4c has very high fusing point, in thermal shock test, can retain good high-temperature stability.
Preferably, described SiC coating and described B
4the thickness proportion of C coating is (3 ~ 8): 1, and described compound coating total thickness is at 150 ~ 200 μm.
Preferably, the thickness of described SiC coating is 60 ~ 160 μm, described B
4the thickness of C coating is 20 ~ 40 μm.
Preferably, described base material is Continuous Fiber Reinforced Ceramic Matrix Composites, is preferably SiC/SiC composite ceramics.
On the other hand, the invention provides above-mentioned high temperature resistant anti-thermal shock SiC/B
4the preparation method of C compound coating, comprises the following steps:
(1) base material to be deposited is carried out high-temperature heat treatment;
(2) thermal treatment terminate after at substrate material surface by chemical vapor deposition SiC coating;
(3) chemical vapor deposition B is passed through at the SiC coating outer surface of gained
4c coating.
The present invention adopts chemical vapor deposition method to prepare coating at substrate material surface, the method film deposition system is simple, the generally easy acquisition of reaction source material needed for film forming, in coating preparation process, material just can continuous production different coating without the need to taking out, preparation coating uniform and there is good density, particularly be applicable at complex-shaped material surface and inner plated film, this method has the features such as simple to operate, film formation time is short, repeatability is strong, is a kind of method having operability.
Preferably, in step (1), described high-temperature heat treatment is carried out in protective atmosphere, and thermal treatment temp is 1200 DEG C ~ 1600 DEG C, and heat treatment time is 1 ~ 2 hour.
Preferably, in step (2), take hydrogen as carrier gas, be brought in cvd furnace by Bubbling method by trichloromethyl silane, carrier gas flux is 400 ~ 800ml/min, be simultaneously diluent gas with argon gas, diluting gas flow is 200 ~ 800ml/min, and the mol ratio of hydrogen and trichloromethyl silane is 10:1 ~ 20:1, and depositing temperature is 850 DEG C ~ 1100 DEG C, pressure is 10 ~ 20KPa, and depositing time is 4 ~ 20 hours.
Preferably, in step (3), gases used is ethene, BCl
3and hydrogen, argon gas is diluent gas, ethene, BCl
3be respectively 250 ~ 450ml/min and 500 ~ 700ml/min and 1500 ~ 2000ml/min with hydrogen gas flow, diluting gas flow is 600 ~ 1000ml/min, and depositing temperature is 1000 DEG C ~ 1300 DEG C, and pressure is 8 ~ 15KPa, and depositing time is 3 ~ 8 hours.
Preferably, the diluent gas used in step (2) and/or step (3) to be purity be more than 99.999% high-purity argon, the hydrogen purity used is more than 99.99%.
Preferably, before step (1), also comprise the step of substrate material surface polished and cleaned being dried, preferably, polishing sand paper used is 300# ~ 600#; Carry out ultrasonic cleaning with dehydrated alcohol, scavenging period is about 40 minutes; Then dry 2 ~ 3 hours under putting into baking oven 120 DEG C of temperature.
Through SiC/B prepared by method of the present invention
4the fine and close defect of C coating uniform is few, is coated with Coating combination excellent, and repeatedly after thermal shock experiment, coatingsurface is substantially unchanged, and matrix combines closely, shows good thermal shock resistance.The present invention has the advantages such as coat-thickness is controlled, repeatability is strong, simple to operate.
Accompanying drawing explanation
Fig. 1 is the SiC/B adopting chemical vapor deposition method to prepare
4c compound coating is through embodiment 1 thermal shock rear surface light micrograph.As can be seen from the figure the material surface even compact prepared;
Fig. 2 is the SiC/B adopting chemical vapor deposition method to prepare
4c compound coating is through embodiment 2 thermal shock rear surface light micrograph.As can be seen from the figure the material surface even compact prepared;
Fig. 3 is the SiC/B adopting chemical vapor deposition method to prepare
4c compound coating, through embodiment 3 thermal shock rear surface light micrograph, therefrom can be found out, after thermal shock experiment, material surface is still fine and close, only has place's crackle;
Fig. 4 is the SiC/B adopting chemical vapor deposition method to prepare
4c compound coating section light micrograph.As can be seen from the figure two kinds of coatings combine closely.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
One aspect of the present invention provides a kind of high temperature resistant anti-thermal shock SiC/B
4c compound coating.As the base material of this compound coating, include but not limited to Continuous Fiber Reinforced Ceramic Matrix Composites, such as C/C, C/SiC, SiC/SiC composite ceramics etc., compound coating of the present invention is particularly useful for SiC/SiC matrix material.SiC/SiC matrix material due to adopt reinforcement be SiC fiber, so in oxidizing atmosphere can long time use, be applied to the high-technology fields such as aerospace, as being loaded into the oxidation resistant component etc. of atmospheric thermal protection parts, aircraft engine more.Therefore, the present invention can meet the development of Models For Space Science And Technology in recent years to the requirement of material surface thermal protection coating.The difference of thermal expansion coefficients of SiC/SiC matrix material and matrix surface is little, combines closely between coating and matrix.
SiC/B of the present invention
4c compound coating can by SiC and B
4the two-layer composition of C, internal layer is SiC coating, and skin is B
4c coating.The combination of two kinds of coatings not only avoid the oxidized and then loss of strength of material, and both thermal expansivity are suitable, combine firmly between coating.SiC/B
4c coat-thickness ratio can be 3 ~ 8.If ratio is too large, SiC coating is too thick, and coating is easily peeled off, and ratio is too little, and SiC coating is too thin, cannot packing crackle completely.Total coating thickness can be 150 ~ 200 μm.In one example, SiC coat-thickness is about 60 ~ 160 μm.In another example, B
4c coat-thickness is about 20 ~ 40 μm.
In one preferred embodiment, SiC coating and B
4c coating is to be prepared by chemical gaseous phase depositing process.Compound coating even compact defect of the present invention is few, is coated with Coating combination excellent, and repeatedly after thermal shock experiment, coatingsurface is substantially unchanged, and matrix combines closely, shows good thermal shock resistance.
The preparation of compound coating of the present invention can comprise following step:
(1) material surface polished and cleaned to be deposited is dried;
(2) material is put in process stove and carry out high-temperature heat treatment;
(3) thermal treatment deposits SiC coating after terminating in cvd furnace;
(4) then again B is deposited at SiC coating outer surface
4c coating.
In one preferred embodiment, the present invention adopts chemical vapor deposition method to prepare coating at composite material surface, the method film deposition system is simple, the generally easy acquisition of reaction source material needed for film forming, in coating preparation process, material just can continuous production different coating without the need to taking out, preparation coating uniform and there is good density, be particularly applicable at complex-shaped material surface and inner plated film.Exemplarily, the present invention prepares SiC/B
4the specific embodiment of C compound coating can be as described below.
(1) surface treatment: by substrate material surface grinding and polishing to be deposited, polishing sand paper used can be 300# ~ 600#, through dehydrated alcohol ultrasonic cleaning 3 times, each about 40 minutes, then dries, and such as, dries 2 ~ 3 hours at 120 DEG C of temperature.By surface treatment, substrate material surface smooth pieces can be made, be conducive to the deposition of compound coating.But it is above-mentioned to should be understood that surface-treated mode is not limited to.
(2) thermal treatment: the material after drying is put in heat treatment furnace, at Ar or N
2carry out high-temperature heat treatment under protective gas, temperature is 1200 DEG C ~ 1600 DEG C, and heat treatment time is 1 ~ 2 hour.By thermal treatment, before coating preparation, volatile for material internal material pyroprocessing can be fallen, prevent from the process of deposited coatings from having impurity to evaporate causing coating and substrate cannot good combination.
(3) SiC coating preparation: after thermal treatment terminates, by chemical vapor deposition SiC coating.Can the SiC coating of deposition compact by chemical gaseous phase depositing process, and SiC coating is combined closely with matrix.In one example, cvd furnace will be put into through heat treated base material, with ramp to 850 ~ 1100 DEG C of 5 DEG C of per minutes, take hydrogen as carrier gas, by Bubbling method, trichloromethyl silane (MTS) is brought in cvd furnace, carrier gas flux is 400 ~ 800ml/min, be simultaneously diluent gas with argon gas, gas flow is 200 ~ 800ml/min, the mol ratio of hydrogen and MTS is 10:1 ~ 20:1, depositing temperature is 850 DEG C ~ 1100 DEG C, and pressure is 10 ~ 20KPa, and depositing time is 4 ~ 20 hours.SiC coat-thickness is about 60 ~ 160 μm.Coat-thickness can be controlled by the mol ratio of adjustment depositing temperature and hydrogen and MTS.
(4) B
4prepared by C coating: then continue through chemical gaseous phase depositing process and deposit B in SiC coating
4c coating.Therefore in coating preparation process, material just can continuous production different coating without the need to taking out.And obtained B
4c coating has good density, and is combined closely with SiC coating.In one example, move to 1000 ~ 1300 DEG C with the speed of 5 DEG C of per minutes, with ethene, BCl
3be reactant gases with hydrogen, argon gas is diluent gas, ethene, BCl
3250 ~ 450ml/min, 500 ~ 700ml/min and 1500 ~ 2000ml/min is respectively with the gas flow of hydrogen, diluting gas flow is 600 ~ 1000ml/min, depositing temperature is 1000 DEG C ~ 1300 DEG C, pressure is 8 ~ 15KPa, deposits after 3 ~ 8 hours and is down to room temperature taking-up with the speed of 5 DEG C of per minutes.Coat-thickness can be controlled by controlling depositing time, depositing temperature and ethylene gas flow.B
4c coat-thickness is about 20 ~ 40 μm.
The diluent gas purity used in the preparation of two kinds of coatings can be more than 99.999% high-purity argon, hydrogen purity can be more than 99.99%.
Through SiC/B prepared by present method
4the fine and close defect of C coating uniform is few, is coated with Coating combination excellent, and repeatedly after thermal shock experiment, coatingsurface is substantially unchanged, and matrix combines closely, shows good thermal shock resistance.The present invention has the advantages such as coat-thickness is controlled, repeatability is strong, simple to operate.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1: the matrix material of required preparation coating is processed in accordance with the following steps:
(1) by SiC/SiC composite material surface grinding and polishing to be deposited, through dehydrated alcohol ultrasonic cleaning 3 times, each about 40 minutes, then dry;
(2) put in heat treatment furnace by the base material after oven dry, maintaining in-furnace temperature is 1300 DEG C, and under Ar protective gas, carry out high-temperature heat treatment, heat treatment time is 1.5 hours;
(3) sample is put into cvd furnace after terminating by thermal treatment, with the ramp of 5 DEG C of per minutes to depositing temperature 850 DEG C, take hydrogen as carrier gas, be brought in cvd furnace by Bubbling method by trichloromethyl silane (MTS), carrier gas flux is 450ml/min, be simultaneously diluent gas with argon gas, gas flow is 500ml/min, and the mol ratio of hydrogen and trichloromethyl silane is 11:1, and pressure is 18KPa, depositing time is 15 hours, and the thickness of SiC coating is 150 μm;
(4) then with the ramp of 5 DEG C of per minutes to depositing temperature 1150 DEG C, with ethene, BCl
3be reactant gases with hydrogen, argon gas is diluent gas, ethene and BCl
3gas flow is respectively 300ml/min and 600ml/min, and hydrogen flowing quantity is 1600ml/min, and diluting gas flow is 800ml/min, and pressure is 10KPa, deposits after 4 hours and is down to room temperature taking-up with the speed of 5 DEG C of per minutes, B
4the thickness of C coating is 22 μm.
Fig. 4 is SiC/B prepared by the present embodiment
4c compound coating section light micrograph.As can be seen from the figure two kinds of coatings combine closely, and are combined closely with base material.Circulated by the matrix material having deposited coating and be heated to 600 DEG C 3 times, be incubated 5 minutes, put into immediately in room temperature cold water and cool after taking-up, find that coatingsurface there is no and come off, thermal shock performance of coatings is good.Material surface light micrograph after thermal shock as shown in Figure 1, the material surface even compact as can be seen from the figure prepared.
Embodiment 2: the matrix material of required preparation coating is processed in accordance with the following steps:
(1) by SiC/SiC composite material surface grinding and polishing to be deposited, through dehydrated alcohol ultrasonic cleaning 3 times, each about 40 minutes, then dry;
(2) put in heat treatment furnace by the base material after oven dry, maintaining in-furnace temperature is 1300 DEG C, under Ar protective gas, carry out high-temperature heat treatment;
(3) sample is put into cvd furnace after terminating by thermal treatment, with the ramp of 5 DEG C of per minutes to depositing temperature 950 DEG C, take hydrogen as carrier gas, be brought in cvd furnace by Bubbling method by trichloromethyl silane (MTS), carrier gas flux is 450ml/min, be simultaneously diluent gas with argon gas, gas flow is 500ml/min, and the mol ratio of hydrogen and trichloromethyl silane is 11:1, and pressure is 18KPa, depositing time is 15 hours, and the thickness of SiC coating is 153 μm;
(4) then with the ramp to 1150 DEG C of 5 DEG C of per minutes, with ethene, BCl
3be reactant gases with hydrogen, argon gas is diluent gas, ethene and BCl
3gas flow is respectively 300ml/min and 600ml/min, and hydrogen flowing quantity is 1600ml/min, and diluting gas flow is 800ml/min, and pressure is 10KPa, deposits after 4 hours and is down to room temperature taking-up with the speed of 5 DEG C of per minutes, B
4the thickness of C coating is 22 μm.
Circulated by the matrix material having deposited coating and be heated to 800 DEG C 3 times, be incubated 5 minutes, put into immediately in room temperature cold water and cool after taking-up, find that coatingsurface there is no and come off, thermal shock performance of coatings is good.Material surface light micrograph after thermal shock as shown in Figure 2, the material surface even compact as can be seen from the figure prepared.
Embodiment 3: the matrix material of required preparation coating is processed in accordance with the following steps:
(1) by SiC/SiC composite material surface grinding and polishing to be deposited, through dehydrated alcohol ultrasonic cleaning 3 times, each about 40 minutes, then dry;
(2) put in heat treatment furnace by the base material after oven dry, maintaining in-furnace temperature is 1300 DEG C, under Ar protective gas, carry out high-temperature heat treatment;
(3) sample is put into cvd furnace after terminating by thermal treatment, with the ramp to 1050 DEG C of 5 DEG C of per minutes, take hydrogen as carrier gas, be brought in cvd furnace by Bubbling method by trichloromethyl silane (MTS), carrier gas flux is 450ml/min, be simultaneously diluent gas with argon gas, gas flow is 500ml/min, and the mol ratio of hydrogen and trichloromethyl silane is 11:1, and pressure is 18KPa, depositing time is 15 hours, and the thickness of SiC coating is 158 μm;
(4) then with the ramp to 1150 DEG C of 5 DEG C of per minutes, with ethene, BCl
3be reactant gases with hydrogen, argon gas is diluent gas, ethene and BCl
3gas flow is respectively 300ml/min and 600ml/min, and hydrogen flowing quantity is 1600ml/min, and diluting gas flow is 800ml/min, and pressure is 10KPa, deposits after 4 hours and is down to room temperature taking-up with the speed of 5 DEG C of per minutes, B
4the thickness of C coating is 22 μm.
Circulated by the matrix material having deposited coating and be heated to 1000 DEG C 3 times, be incubated 5 minutes, put into immediately in room temperature cold water and cool after taking-up, find that coatingsurface has and slightly come off, thermal shock performance of coatings decreases.Material surface light micrograph after thermal shock as shown in Figure 3, therefrom can be found out, after thermal shock experiment, material surface is still fine and close, only has place's crackle.
Claims (10)
1. a high temperature resistant anti-thermal shock SiC/B
4c compound coating, is characterized in that, comprising: be deposited on the SiC coating on base material and be deposited on the B of SiC coating outer surface
4c coating.
2. high temperature resistant anti-thermal shock SiC/B according to claim 1
4c compound coating, is characterized in that, described SiC coating and described B
4the thickness proportion of C coating is (3 ~ 8): 1, and described compound coating total thickness is at 150 ~ 200 μm.
3. high temperature resistant anti-thermal shock SiC/B according to claim 1 and 2
4c compound coating, is characterized in that, the thickness of described SiC coating is 60 ~ 160 μm, described B
4the thickness of C coating is 20 ~ 40 μm.
4. high temperature resistant anti-thermal shock SiC/B according to any one of claim 1 to 3
4c compound coating, is characterized in that, described base material is Continuous Fiber Reinforced Ceramic Matrix Composites, is preferably SiC/SiC composite ceramics.
5. the high temperature resistant anti-thermal shock SiC/B according to any one of a Claims 1-4
4the preparation method of C compound coating, is characterized in that, comprises the following steps:
(1) base material to be deposited is carried out high-temperature heat treatment;
(2) thermal treatment terminate after at substrate material surface by chemical vapor deposition SiC coating;
(3) chemical vapor deposition B is passed through at the SiC coating outer surface of gained
4c coating.
6. preparation method according to claim 5, is characterized in that, in step (1), described high-temperature heat treatment is carried out in protective atmosphere, and thermal treatment temp is 1200 DEG C ~ 1600 DEG C, and heat treatment time is 1 ~ 2 hour.
7. the preparation method according to claim 5 or 6, it is characterized in that, in step (2), take hydrogen as carrier gas, by Bubbling method, trichloromethyl silane is brought in cvd furnace, carrier gas flux is 400 ~ 800ml/min, and be simultaneously diluent gas with argon gas, diluting gas flow is 200 ~ 800ml/min, the mol ratio of hydrogen and trichloromethyl silane is 10:1 ~ 20:1, depositing temperature is 850 DEG C ~ 1100 DEG C, and pressure is 10 ~ 20KPa, and depositing time is 4 ~ 20 hours.
8. the preparation method according to any one of claim 5 to 7, is characterized in that, in step (3), gases used is ethene, BCl
3and hydrogen, argon gas is diluent gas, ethene, BCl
3be respectively 250 ~ 450ml/min, 500 ~ 700ml/min and 1500 ~ 2000ml/min with hydrogen gas flow, diluting gas flow is 600 ~ 1000ml/min, and depositing temperature is 1000 DEG C ~ 1300 DEG C, and pressure is 8 ~ 15KPa, and depositing time is 3 ~ 8 hours.
9. preparation method according to claim 8, is characterized in that, the diluent gas used in step (2) and/or step (3) to be purity be more than 99.999% high-purity argon, the hydrogen purity used is more than 99.99%.
10. the preparation method according to any one of claim 5 to 9, is characterized in that, before step (1), also comprises the step of substrate material surface polished and cleaned being dried, and preferably, polishing sand paper used is 300# ~ 600#; Carry out ultrasonic cleaning with dehydrated alcohol, scavenging period is about 40 minutes; Then dry 2 ~ 3 hours under putting into baking oven 120 DEG C of temperature.
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