CN108516833A - Powder, coating and preparation method for ceramic matric composite high-temperature oxidation resistant - Google Patents
Powder, coating and preparation method for ceramic matric composite high-temperature oxidation resistant Download PDFInfo
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Abstract
For the powder, coating and preparation method of ceramic matric composite high-temperature oxidation resistant, belong to high-temperature protection coating field.A kind of fine and close SiC coatings with certain content free silica suitable for C/C either B, Ta or B of C/SiC ceramic matric composites, La or B, Mo codope are prepared using high temperature solid state diffusion technique.Free silica is 3~25wt.% in the coating, and B is 0.1~2wt.%, and either La or Mo is 0.1~2.5wt.%, surplus SiC to Ta.B is generated in oxidation process by adding B2O3With lower fusing point (450 DEG C) and good mobility, realize the self-healing anti-oxidation of material, add infusibility phase and the Ta of corresponding oxide also infusibility either La or Mo can reduce diffusion velocity of the oxygen in oxidation film, inhibit oxygen inwardly to spread.This novel co-doping method significantly improves SiC coating high temperature oxidation resistances.
Description
Technical field
The invention belongs to high-temperature protection coating fields, are related to a kind of powder for ceramic matric composite high-temperature oxidation resistant
End, coating and preparation method, more specifically refer to using powder metallurgy solid state diffusion sintering process prepare it is a kind of be suitable for C/SiC or
Powder, coating and the preparation method of C/C ceramic matric composite high-temperature oxidation resistants.
Background technology
Ceramic matric composite has the characteristics that hardness is high, density is small, coefficient of thermal expansion is low and mechanical behavior under high temperature is excellent,
But the problem of easily being aoxidized in high temperature aerobic environment seriously limits its application as high-temperature structural material.In composite wood
It is a kind of effective ways for improving its high temperature antioxygen property that material surface, which prepares high-temperature oxidation resistant coating,.SiC has good chemistry
Stability and excellent high-temperature oxidation resistant characteristic and compatible with the relatively good physical chemistry of C/SiC and C/C composite materials
Property, it is the ideal coating material of ceramic matric composite.
Li He armies et al. are prepared for SiC high-temperature oxidation resistant coatings, but As-deposited state using investment in C/C composite material surfaces
Coating surface there are fine crack, crack width is 1~3 micron, and there are through wall flaws for coating.It is aoxidized through 1500 DEG C
Many spileholes are formed in the oxidation film generated afterwards, these stomatas are that oxygen enters C/C composite inners under hot environment
Main thoroughfare.(see reference document 1：Sun Guodong, Li Hejun, Fu Qiangang, Zhang Yulei, Li Kezhi, the C/C with SiC coatings are compound
The oxidation behavior solid-rocket technologies of material, 2010,33 (1):91-94).
Yulei Zhang et al. have studied a kind of method that pre- carbon-coating is added to prepare gradient transition SiC coatings, this kind applies
Layer reduces the thermal expansion between coating and matrix and mismatches to a certain extent, but the high-temperature oxidation resistance of coating is not
It is significantly improved.(see reference document 2：Yulei Zhang,Hejun Li,Kezhi Li.A C/SiC gradient
oxidation protective coating for carbon/carbon composition.Surface and
Coatings Technology,2006(201):3491-3495)。
SiC coating existing defects prepared by the above method are more, the problem of antioxygenic property deficiency.Coating crack and defect are
The main reason for compound material antioxygenic property is poor.SiC coatings have 1700 DEG C to ceramic matric composite in theory to be prevented
Shield ability, but due to the difference of coefficient of thermal expansion between SiC coatings and matrices of composite material, coating is easy to crack, the crackle of generation
The antioxygenic property of single SiC coatings can be seriously affected, in addition SiC coatings during oxidation due to the generation of gas aoxidize
Can there are Minute pores, micro-crack and hole in film and provide channel for the diffusion of oxygen, cause the antioxygenic property of coating insufficient.
Therefore, it is used for 1650 DEG C of long-lives of realization ceramic matric composite, it is necessary to improve its high-temperature oxidation resistance.
Invention content
The purpose of the invention is to overcome the shortcomings of original technology, provide first a kind of high for ceramic matric composite
The oxidation resistant powder of temperature, chemical composition are：Si 3~25wt.%, B 0.1~2wt.%, Ta either La or Mo 0.1~
2.5wt.%, surplus SiC.
The present invention also provides a kind of methods preparing the powder for ceramic matric composite high-temperature oxidation resistant, will be high-purity
Either dispensing mixes La Mo powder in proportion by SiC powder, Si powder, B powder and Ta, wet after addition organic liquid into mixed-powder
Method ball milling disperses, and the slurry drying after ball milling is disperseed obtains the powder for ceramic matric composite high-temperature oxidation resistant.It is organic
Liquid is the conventional ball mills organic liquids such as acetone, ethyl alcohol, and ball-milling medium and ball grinder material select conventional material, not introduce
Subject to impurity.
Further, for the SiC powder purities 99.9% or more, granularity is 30~50 μm；Si powder purities 99.9% with
On, granularity is 30~50 μm；For B powder purities 99.9% or more, granularity is 1~30 μm；Either La Mo powder purities exist Ta
99.9% or more, granularity is 1~30 μm.
The present invention also provides a kind of coating for ceramic matric composite high-temperature oxidation resistant, the content of free silica in coating
For 3~25wt.%, the content of B is 0.1~2wt.%, and the content of Ta either La or Mo is 0.1~2.5wt.%, and surplus is
SiC。
Further, coating layer thickness is 50~150 μm.
The present invention also provides a kind of methods preparing the coating for ceramic matric composite high-temperature oxidation resistant, more specifically
Refer to preparing one kind using powder metallurgy solid state diffusion sintering process combination plasma sintering process to be suitable for C/SiC or C/C ceramics
The method of composite material high-temperature oxidation resistant coating.It is multiple in C/SiC C/C ceramics first with powder metallurgy solid state diffusion sintering process
Condensation material matrix surface prepare one layer 50~150 μm B, Ta either B, La or B, Mo codopes it is free with certain content
Then the fine and close SiC coatings of silicon carry out plasma agglomeration processing to the coating of preparation.The preparation method includes the following steps：
(1) basis material pre-processes：Ceramic matric composite matrix is cut into sample, the sample cut is polished, will be beaten
The matrix sample of milled is cleaned by ultrasonic, and is dried for standby；
(2) sintered material prepares：It is added into sintering vessel anti-provided by the present invention for ceramic matric composite high temperature
The powder of oxidation is then placed in step (1) pretreated sample, is then added again multiple provided by the present invention for ceramic base
The powder of condensation material high-temperature oxidation resistant fills up sintering vessel, and gently powder compaction excludes the air in sintering vessel, will be sintered
Vessel are closed；
(3) high temperature solid state diffusion is sintered：Step (2) ready sintering vessel is put into vacuum sintering furnace, sintering furnace is taken out true
Sky is to air pressure 2 × 10-2For Pa hereinafter, heating temperature is to 1700 DEG C~2100 DEG C, soaking time is 1~4 hour；Wait for vacuum-sintering
Stove, which is cooled to room temperature, takes out the sample prepared, is dried after ultrasonic cleaning；
(4) plasma agglomeration：The sample coatings that step (3) is obtained carry out plasma agglomeration processing, plasma agglomeration work
Skill parameter is：The sintering rate of 800~1200 DEG C/min keeps the temperature 20~40min after rising to 1700~1900 DEG C.Purpose is to reduce
Holiday, solidification interface combine, and reduce matrix oxidation, and modified SiC of the present invention is obtained after plasma agglomeration processing and is applied
Layer.
Further, the ceramic matric composite matrix described in step (1) is that C/SiC ceramic composites or C/C are multiple
Condensation material.
Further, the sintering vessel described in step (3) is boron nitride crucible.
Further, 60~80% that amount of powder is sintering vessel volume are added in step (3) for the first time.
The SiC coatings being prepared by the above method, the oxygen after atmospheric environment high temperature cyclic oxidation 10h at 1500 DEG C
Change weight loss and is no more than 4.9%.
The coating for ceramic matric composite high-temperature oxidation resistant prepared by the present invention has the following advantages：
Due to the difference of coefficient of thermal expansion between SiC coatings and matrices of composite material, so that coating is inevitably present and split
Line, and SiC oxidations generate SiO2Speed it is slow, poor fluidity, it is difficult to which the crackle in packing coating causes oxygen to be easy to diffuse to
Intrinsic silicon.B is generated in oxidation process by adding B2O3It, can with lower fusing point (450 DEG C) and good mobility
Crackle in healing coating prevents oxygen from being spread to material internal by micro-crack, realizes the self-healing anti-oxidation of material, effectively carry
The high high temperature oxidation resistance of SiC coatings.By added into SiC coatings infusibility phase, corresponding oxide also the Ta of infusibility or
Person La or Mo can reduce diffusion velocity of the oxygen in oxidation film, the SiO for inhibiting oxygen inwardly to spread, and being formed2Protective layer
It is more fine and close.This novel B, Ta either B, La or B, Mo codope SiC coating high-temp antioxygenic properties be substantially better than it is general
Logical SiC coatings, effectively increase the service life of coating.
Description of the drawings
Fig. 1 is the surface topography map of modified SiC high-temperature oxidation resistant coatings provided by the invention.
Fig. 2 is the Cross Section Morphology figure of modification SiC high-temperature oxidation resistant coatings prepared by the present invention.
Fig. 3 is the surface topography map after 1500 DEG C of oxidation 10h of modification SiC high-temperature oxidation resistant coatings prepared by the present invention.
Specific implementation mode
The present invention is described in detail with reference to the accompanying drawings and examples.
Embodiment 1：Modified SiC high-temperature oxidation resistant coatings are prepared on C/SiC matrices of composite materials
The first step：Prepare basis material
Ceramic matric composite matrix is cut into the sample that specification is 10 × 10 × 3mm, then by the sample cut through sand
Paper is polished, and 12 ribs are all changed into fillet, finally uses the matrix sample polished successively absolute ethyl alcohol and acetone ultrasound clear
Wash 15 minutes, 120 DEG C dry 2 hours, it is spare.The ceramic matric composite matrix chooses C/SiC ceramic composites.
Second step：Prepare penetrant powder
(granularity is for the SiC powder for the use of purity being 99.9% (granularity is 30~50 μm), the Si powder that purity is 99.9%
30~50 μm), the B powder (granularity is 1~10 μm) that purity is 99.9% and Ta powder that purity is 99.9% (granularity is 1~
10 μm) it is raw material.Prepared penetration enhancer chemical composition is that SiC content is 84wt.%, and Si contents are 15wt.%, and the content of B is
The content of 0.5wt.%, Ta are 0.5wt.%.Prepared powder is placed in resin ball grinder and acetone ball milling is added 10 hours,
Mixed liquor taking-up is placed at 100 DEG C and dries, is spare.
Third walks：On matrix modified SiC coatings are prepared using powder metallurgy solid state diffusion sintering process
The penetrant powder of 70% volume, the matrix that then will prepare in the first step is added into 5ml boron nitride crucibles first
Sample is put among the boron nitride crucible that penetrant powder has been added, and is then again filled up crucible with penetrant powder, and sample is wrapped
Among penetrant powder, gently powder compaction excludes the air in crucible, and crucible lid is covered tightly.Crucible equipped with sample is put
Enter in vacuum sintering furnace, sintering furnace is evacuated to vacuum degree and is less than 2 × 10-2Pa, heating temperature is to 1800 DEG C, soaking time 2
Hour, alloying layer thickness is~90 μm；It waits for that vacuum sintering furnace is cooled to room temperature to take out the coating sample prepared, with acetone ultrasound
It is dried after cleaning 15min.
4th step：The coating of preparation is subjected to plasma agglomeration processing
Plasma sintering process parameter is：The sintering rate of 1100 DEG C/min keeps the temperature 30min, after plasma agglomeration processing
Obtain modified SiC coatings of the present invention.
Modification SiC coating structures prepared by the above method are fine and close, plasma agglomeration treated coating morphology and cut
Face pattern is as shown shown in Figure 1 and Figure 2, in 1500 DEG C of atmospheric environments after cyclic oxidation 10h, observes the surface shape of sample
Looks, the oxidation film that modified SiC coating surfaces generate is completely fine and close, and it is 4.8% to aoxidize the oxidation weight loss after 10h, illustrates to be modified
SiC coating high-temp antioxygenic properties are preferable.
Embodiment 2：Modified SiC high-temperature oxidation resistant coatings are prepared on C/C matrices of composite materials
The first step：Prepare basis material
Ceramic matric composite matrix is cut into the sample that specification is 10 × 10 × 3mm, then by the sample cut through sand
Paper is polished, and 12 ribs are all changed into fillet, finally uses the matrix sample polished successively absolute ethyl alcohol and acetone ultrasound clear
Wash 15 minutes, 120 DEG C dry 2 hours, it is spare.The ceramic matric composite matrix chooses C/C ceramic composites.
Second step：Prepare penetrant powder
(granularity is for the SiC powder for the use of purity being 99.9% (granularity is 30~50 μm), the Si powder that purity is 99.9%
30~50 μm), the B powder (granularity is 1~30 μm) that purity is 99.9% and La powder that purity is 99.9% (granularity is 1~
30 μm) it is raw material.Prepared penetration enhancer chemical composition is that SiC content is 84wt.%, and Si contents are 15wt.%, and the content of B is
The content of 0.5wt.%, La are 0.5wt.%.Prepared powder is placed in resin ball grinder and acetone ball milling is added 10 hours,
Mixed liquor taking-up is placed at 100 DEG C and dries, is spare.
Third walks：On matrix modified SiC coatings are prepared using powder metallurgy solid state diffusion sintering process
The penetrant powder of 70% volume, the matrix that then will prepare in the first step is added into 5ml boron nitride crucibles first
Sample is put among the boron nitride crucible that penetrant powder has been added, and is then again filled up crucible with penetrant powder, and sample is wrapped
Among penetrant powder, gently powder compaction excludes the air in crucible, and crucible lid is covered tightly.Crucible equipped with sample is put
Enter in vacuum sintering furnace, sintering furnace is evacuated to vacuum degree and is less than 2 × 10-2Pa, heating temperature is to 1900 DEG C, soaking time 2
Hour, alloying layer thickness is~100 μm；It waits for that vacuum sintering furnace is cooled to room temperature to take out the coating sample prepared, it is super with acetone
It is dried after sound cleaning 15min.
4th step：The coating of preparation is subjected to plasma agglomeration processing
Plasma sintering process parameter is：The sintering rate of 1000 DEG C/min keeps the temperature 30min after rising to 1800 DEG C, wait from
Modified SiC coatings of the present invention are obtained after sub- sintering processes.
Modification SiC coating structures prepared by the above method are fine and close, and by plasma agglomeration, treated that sample is big at 1500 DEG C
In compression ring border after cyclic oxidation 10h, the surface topography of sample is observed, the oxidation film that modified SiC coating surfaces generate completely causes
Close, it is 4.9% to aoxidize the oxidation weight loss after 10h, illustrates that modified SiC coating high-temp antioxygenic properties are preferable.
Embodiment 3：Modified SiC high-temperature oxidation resistant coatings are prepared on C/SiC matrices of composite materials
The first step：Prepare basis material
Ceramic matric composite matrix is cut into the sample that specification is 10 × 10 × 3mm, then by the sample cut through sand
Paper is polished, and 12 ribs are all changed into fillet, finally uses the matrix sample polished successively absolute ethyl alcohol and acetone ultrasound clear
Wash 15 minutes, 120 DEG C dry 2 hours, it is spare.The ceramic matric composite matrix chooses C/C ceramic composites.
Second step：Prepare penetrant powder
(granularity is for the SiC powder for the use of purity being 99.9% (granularity is 30~50 μm), the Si powder that purity is 99.9%
30~50 μm), the B powder (granularity is 1~30 μm) that purity is 99.9% and La powder that purity is 99.9% (granularity is 1~
30 μm) it is raw material.Prepared penetration enhancer chemical composition is that SiC content is 84wt.%, and Si contents are 15wt.%, and the content of B is
The content of 0.5wt.%, Mo are 0.5wt.%.Prepared powder is placed in resin ball grinder and acetone ball milling is added 10 hours,
Mixed liquor taking-up is placed at 100 DEG C and dries, is spare.
Third walks：On matrix modified SiC coatings are prepared using powder metallurgy solid state diffusion sintering process
The penetrant powder of 70% volume, the matrix that then will prepare in the first step is added into 5ml boron nitride crucibles first
Sample is put among the boron nitride crucible that penetrant powder has been added, and is then again filled up crucible with penetrant powder, and sample is wrapped
Among penetrant powder, gently powder compaction excludes the air in crucible, and crucible lid is covered tightly.Crucible equipped with sample is put
Enter in vacuum sintering furnace, sintering furnace is evacuated to vacuum degree and is less than 2 × 10-2Pa, heating temperature is to 2000 DEG C, soaking time 2
Hour, alloying layer thickness is~120 μm；It waits for that vacuum sintering furnace is cooled to room temperature to take out the coating sample prepared, it is super with acetone
It is dried after sound cleaning 15min.
4th step：The coating of preparation is subjected to plasma agglomeration processing
Plasma sintering process parameter is：The sintering rate of 1000 DEG C/min keeps the temperature 30min after rising to 1800 DEG C, wait from
Modified SiC coatings of the present invention are obtained after sub- sintering processes.
Modification SiC coating structures prepared by the above method are fine and close, and by plasma agglomeration, treated that sample is big at 1500 DEG C
In compression ring border after cyclic oxidation 10h, the surface topography of sample is observed, the oxidation film that modified SiC coating surfaces generate completely causes
Close, it is 4.7% to aoxidize the oxidation weight loss after 10h, illustrates that modified SiC coating high-temp antioxygenic properties are preferable.
Claims (9)
1. the powder for ceramic matric composite high-temperature oxidation resistant, which is characterized in that powder chemistry ingredient is：Si 3~
25wt.%, B 0.1~2wt.%, Ta either 0.1~2.5wt.% of La or Mo, surplus SiC.
2. the preparation method of powder described in claim 1, which is characterized in that by high-purity alpha-SiC powder, Si powder, B powder and Ta or La
Or dispensing mixes Mo powder in proportion, wet ball grinding disperses after organic liquid is added into mixed-powder, after ball milling is disperseed
Slurry is dried, and the powder for ceramic matric composite high-temperature oxidation resistant is obtained.
3. preparation method according to claim 2, which is characterized in that the SiC powder purities are in 99.9% or more, granularity
30~50 μm；For Si powder purities 99.9% or more, granularity is 30~50 μm；For B powder purities 99.9% or more, granularity is 1~30 μ
m；Either for La Mo powder purities 99.9% or more, granularity is 1~30 μm to Ta.
4. for ceramic matric composite high-temperature oxidation resistant coating, which is characterized in that in coating the content of free silica be 3~
The content of 25wt.%, B be 0.1~2wt.%, Ta either La or Mo content be 0.1~2.5wt.%, surplus SiC.
5. coating according to claim 4, which is characterized in that coating layer thickness is 50~150 μm.
6. the preparation method of the coating described in claim 4 or 5, which is characterized in that include the following steps：
(1) basis material pre-processes：Ceramic matric composite matrix is cut into sample, the sample cut is polished, will be polished
Matrix sample be cleaned by ultrasonic, be dried for standby；
(2) sintered material prepares：Powder described in claim 1 is added into sintering vessel, is then placed in step (1) pretreatment
Then sample afterwards is added powder described in claim 1 and fills up sintering vessel again, powder compaction excludes in sintering vessel
Air, sintering vessel is closed；
(3) high temperature solid state diffusion is sintered：Step (2) ready sintering vessel is put into vacuum sintering furnace, sintering furnace is evacuated to
Air pressure is 2 × 10-2For Pa hereinafter, heating temperature is to 1700 DEG C~2100 DEG C, soaking time is 1~4 hour；Wait for that vacuum sintering furnace drops
The sample prepared is taken out after to room temperature, is dried after ultrasonic cleaning；
(4) plasma agglomeration：The sample coatings that step (3) is obtained carry out plasma agglomeration processing, plasma sintering process ginseng
Number is：The sintering rate of 800~1200 DEG C/min keeps the temperature 20~40min after rising to 1700~1900 DEG C.
7. preparation method according to claim 6, which is characterized in that the ceramic matric composite matrix described in step (1)
For C/SiC ceramic composites or C/C composite materials.
8. preparation method according to claim 6, which is characterized in that the sintering vessel described in step (3) is boron nitride earthenware
Crucible.
9. preparation method according to claim 6, which is characterized in that it is sintering that amount of powder is added in step (3) for the first time
The 60~80% of vessel volume.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810350882.2A CN108516833B (en) | 2018-04-18 | 2018-04-18 | High-temperature oxidation-resistant powder and coating for ceramic matrix composite and preparation method thereof |
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|---|---|---|---|
| CN201810350882.2A CN108516833B (en) | 2018-04-18 | 2018-04-18 | High-temperature oxidation-resistant powder and coating for ceramic matrix composite and preparation method thereof |
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| Publication Number | Publication Date |
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| CN108516833A true CN108516833A (en) | 2018-09-11 |
| CN108516833B CN108516833B (en) | 2020-04-14 |
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| CN110124526A (en) * | 2019-04-30 | 2019-08-16 | 湖北工业大学 | A kind of production method of silicon carbide inorganic ceramic membrane |
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| CN102432345A (en) * | 2011-09-22 | 2012-05-02 | 中南大学 | Carbon/carbon composite material silicon-based composite coating capable of resisting high-temperature oxidation for long time, and its preparation method and use |
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| CN102432345A (en) * | 2011-09-22 | 2012-05-02 | 中南大学 | Carbon/carbon composite material silicon-based composite coating capable of resisting high-temperature oxidation for long time, and its preparation method and use |
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| S. BURK ET AL.: ""Oxidation Behavior of Mo-Si-B-(X) Alloys: Macro- and Microalloying (X= Cr, Zr, La2O3)", 《JOM》 * |
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| CN110124526A (en) * | 2019-04-30 | 2019-08-16 | 湖北工业大学 | A kind of production method of silicon carbide inorganic ceramic membrane |
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