CN105198501B - A kind of preparation method of surface of carbon/carbon composite tungsten gradient coating - Google Patents
A kind of preparation method of surface of carbon/carbon composite tungsten gradient coating Download PDFInfo
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- CN105198501B CN105198501B CN201510655207.7A CN201510655207A CN105198501B CN 105198501 B CN105198501 B CN 105198501B CN 201510655207 A CN201510655207 A CN 201510655207A CN 105198501 B CN105198501 B CN 105198501B
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Abstract
The present invention relates to a kind of preparation method of surface of carbon/carbon composite tungsten gradient coating, for C/C composites and W poor compatibilities, the problems such as easily generating WC brittlement phases, the inventive method prepares SiC/WSi in C/C composite material surfaces using two investments in advance2Transition zone improves C/C composites and metal W physical chemistry compatibility transition zone, is finally having SiC/WSi using the success of Supersonic Plasma Spraying technique2The C/C composite material surfaces of transition zone prepare W coatings, so as to prepare C Si W gradient coatings in C/C composite material surfaces.SiC/WSi2Transition zone and spraying W external coatings self structure are fine and close, are firmly combined with matrix, and the C/C composites that preparing has C Si W gradient coatings keep the excellent properties such as self-strength is high, proportion is small, while can possess the excellent properties of metal W.
Description
Technical field
The invention belongs to carbon/carbon compound material coating preparation field, and in particular to a kind of surface of carbon/carbon composite metal
The preparation method of tungsten gradient coating.
Background technology
Carbon/carbon (C/C) composite has an a series of incomparable excellent properties of other materials, such as low-density, than strong
Spend high, the peculiar high-temperature mechanics strength retention of big high, specific modulus, anti-yaw damper, rub resistance, heat shock resistance, damage tolerance and good
Good designability, either applied to field of aerospace, core field, biomedical and vehicle electric field etc., C/C is multiple
Condensation material all shows huge application prospect.Yet with the unique preparation technology and Carbon Materials itself of C/C composites
Structure, the limitation of aspect of performance so that the shortcoming that some can not overcome itself occur in C/C composites, such as high-temperature oxidation resistant is poor,
Burning corrosion resistance can be not enough, not a series of problems, such as erosion resistance.Tungsten (W) is to be currently known fusing point highest metal, and is had
There are the characteristics such as high intensity, high elastic modulus, low thermal coefficient of expansion, be good anti-yaw damper material, the tungsten studied around metal W oozes
Copper, tungsten ooze the tungsten alloys such as silver and have been widely used in the fields such as Aero-Space engine jet pipe, guided missile jet vane.Such as patent 1
“Advanced Materials and Processes for Boost Phase Nozzles,Robert Hickman,
PPI companies are prepared for W-Re and W-Re-HfC dead sizes using vacuum plasma spray coating technique in Timothy McKechnie. "
Jet pipe, (aluminized propellant, 3000 DEG C of operating pressure 9MPa, temperature, working time are examined through solid propellant rocket heat run>
2.5s), throat ablative rate is zero, shows that metal W has extremely strong anti-yaw damper ability.But W density is too high, which has limited it
The research of W coatings is prepared in the application of field of aerospace, therefore on the surface of low-density C/C composites, is expected to combine two
The advantage of person prepares the material of more preferable performance.It is plasma spraying, supersonic speed that W coatings, which prepare most ripe also the most frequently used technology,
Plasma spraying compared with other hot-spraying technique flying speed of partcles faster, melts more abundant, therefore gained anchoring strength of coating is more
Height, it is also finer and close.Mismatched yet with W and C/C Thermal expansion coefficient of composites, and physical chemistry compatibility is poor, C/C is multiple
Condensation material surface W coatings prepare difficulty, and the bond strength of coating and matrix is undesirable, on the other hand, and W easily reacts with C
Generation tungsten carbide (WC) brittlement phase causes the failure of coating." the Behavior of plasma-sprayed tungsten of document 1
Coatings on CFC and graphite under high heat load, K.Tokunaga, N.Yoshida,
N.Noda, Y.Kubota, S.Inagaki " go out multilayer rhenium (Re) in CFC composites and graphite surface using PVD deposition respectively
With the transition zone of tungsten (W), W coatings are then prepared using plasma spraying.But process complexity is this method increased, make into
Originally greatly improve.Therefore W coatings are prepared in C/C composite material surfaces at present and also there are many difficult points.
The content of the invention
The technical problem to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of surface of carbon/carbon composite tungsten gradient
The preparation method of coating.
Technical scheme
A kind of preparation method of surface of carbon/carbon composite tungsten gradient coating, it is characterised in that step is as follows：
Step 1, pretreatment C/C composites：Carbon/carbon C/C composites polishing is allowed to surface roughening, then distinguished
It is cleaned by ultrasonic with water and absolute ethyl alcohol, is placed in air and dries or oven for drying；
Step 2：By Si powder, C powder, Al2O3Powder is well mixed, made according to 65-80%, 10-25%, 5-15% mass ratio
It is put into for embedding powder in graphite crucible, step 1 is pre-processed in C/C composites embedment powder, it is compound in carbon/carbon C/C
Material surface prepares SiC/Si transition zones；
Crucible is put into high-temperature vacuum graphitizing furnace under argon atmosphere, 1800~2000 DEG C of insulation 2h are had
There are the C/C composites of SiC coatings, then make coating surface smooth with sand paper polishing, and be cleaned and dried；
Step 3：By 40-60% Si powder, 30-50% C powder, the mass ratio of 5-15% W powder is well mixed, and is used as bag
Buried powder material is put into graphite crucible, and the C/C composites with SiC coatings that step 2 is obtained are embedded in powder；
Crucible is put into high-temperature vacuum graphitizing furnace under argon atmosphere, 2000~2200 DEG C of insulation 2h are had
There is SiC/WSi2The C/C composites of transition zone, then make coating surface smooth, and be cleaned and dried with sand paper polishing；
Step 4：PVA and water are pressed 1:7 ratio dissolves in 100 DEG C of constant water bath box is hybridly prepared into PVA glues, will
Metal W powder is with PVA colloidal sols with 1:Uniform suspension is formed after 1 mass ratio mixing, ultrasonic disperse 30min, and is carried out at granulation
Reason, obtains 30~50um of diameter ball-type W spraying powders；
Step 5：Using ball-type W powders as spraying powder, using HEPJ type Supersonic Plasma Spraying equipment in SiC/WSi2
Internally coated C/C composite material surfaces W coatings, complete the preparation of surface of carbon/carbon composite tungsten gradient coating；It is described
Spraying coating process is as follows：Spray power 50-60KW, primary air amount 70-80L/min, powder sending quantity 3.5-4.5r/min, nozzle tip are arrived
Specimen surface is apart from 10-13cm.
The polishing of the step 1 uses 80 mesh coarse sandpapers.
Being cleaned by ultrasonic with water and absolute ethyl alcohol for the step 1 is 5-10min.
The granulation processing of the step 4 carries out granulation processing using LGZ-5 sponging granulators to powder.
Beneficial effect
A kind of preparation method of surface of carbon/carbon composite tungsten gradient coating proposed by the present invention, it is compound for C/C
The problems such as material and W poor compatibilities, easily generation WC brittlement phases, the inventive method uses two in C/C composite material surfaces in advance
Investment prepares SiC/WSi2Transition zone improves C/C composites and metal W physical chemistry compatibility transition zone, finally uses
The success of Supersonic Plasma Spraying technique is having SiC/WSi2The C/C composite material surfaces of transition zone prepare W coatings, so that in C/
Prepare C-Si-W gradient coatings in C composite surface.SiC/WSi2Transition zone and spraying W external coatings self structure are fine and close, with
Matrix is firmly combined with, and the C/C composites that preparing has C-Si-W gradient coatings keep the superiority such as self-strength is high, proportion is small
Can, while the excellent properties of metal W can be possessed.
The present invention prepares SiC/WSi using two investments2Transition zone improves C/C composites and metal W is physico
Compatibility is learned, the bond strength of plasma spraying external coating and matrix is improved, and can also suppress W's and C as barrier layer
Diffusion reaction, prevents the generation of WC brittlement phases during use.Metal W powder is bought to market to carry out the processing of granulation ball-typeization to increase
Plus powder mobility is so as to improve spraying effect.The W external coating compact structures finally prepared using Supersonic Plasma Spraying, nothing
Obvious hole and penetrating crack.C-Si-W gradient coatings are integrally well combined with C/C matrices of composite materials, are answered keeping C/C
Possess the excellent properties of metal W while the excellent properties such as condensation material self-strength is high, proportion is small.
The prepares coating performance of the present invention is remarkable, equipment requirement is not high, and process parameter control is simple, and to material surface
Regular shape without particular/special requirement, there is low cost, pollute small and easily realize that scale efficiency is produced, with aobvious
The economic and social benefit of work.
Brief description of the drawings
Fig. 1：C/C composite material surfaces SiC/WSi prepared by embodiment 32Transition layer surface SEM photograph；
Fig. 2：C/C composite material surfaces SiC/WSi prepared by embodiment 32Transition layer cross section SEM photograph；
Fig. 3：C/C composite material surface SiC/WSi2 transition layer surface XRD spectrums prepared by embodiment 3；
Fig. 4：C/C composite material surface C-Si-W gradient coatings outer surface SEM photograph prepared by embodiment 3；
Fig. 5：C/C composite material surface C-Si-W gradient coatings section SEM photograph prepared by embodiment 3；
Fig. 6：C/C composite material surface C-Si-W gradient coatings surface XRD spectrum prepared by embodiment 3.
Embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described：
Embodiment one：
1) it is ρ=1.70g/cm by density by 10 × 10 × 10mm specifications3C/C composite processing into sample, use
The polishing of 80 mesh coarse sandpapers is allowed to surface roughening, is dried after cleaning；
2) Si powder, C powder, Al are bought with market2O3Powder is that raw material presses 6:1:0.8 ratio mixing, then puts mixed-powder
0.5h is stirred in ball blending machine, embedding powder is used as.Step 1 gained C/C samples are put into graphite crucible, and are embedded to above-mentioned powder
Material.Crucible is put into high-temperature vacuum graphitizing furnace under argon atmosphere, 1800 DEG C of insulation 2h must can have certain thickness
The C/C composite samples of SiC/Si coatings.Then make coating surface smooth with sand paper polishing, be cleaned and dried；
3) Si powder, W powder are bought with market, C powder is that raw material presses 6:6:1 ratio mixing, is then placed in ball by mixed-powder
0.5h is stirred in type mixer, embedding powder is used as.The C/C samples for there are SiC/Si coatings obtained by step 2 are put into graphite crucible, and
It is embedded to above-mentioned powder.Crucible is put into high-temperature vacuum graphitizing furnace under argon atmosphere, 2100 DEG C of insulation 2h can must have one
Determine the SiC/WSi of thickness2The C/C composite samples of coating.Then make coating surface smooth with sand paper polishing, be cleaned and dried；
4) PVA and water are pressed 1:7 ratio dissolves to be well mixed in 100 DEG C of constant water bath box is configured to PVA glues, will
Market is bought metal W powder and is mixed into wherein, and uniform suspension is formed after ultrasonic disperse 30min.Using LGZ-5 sponging granulators to original
Powder carries out granulation processing, obtains diameter 40um or so ball-type W spraying powders；
5) HEPJ type Supersonic Plasma Spraying equipment is used, is there is SiC/WSi2The C/C composite samples of transition zone
Surface is with power 50KW, powder sending quantity 4.0r/min, is prepared under primary air amount 77.4L/min spray parameters outside 50um or so W
Coating；
Prepared SiC-SiC/WSi of the invention2Transition zone and W external coatings are comparatively dense, and external coating voidage≤
2%, coating surface is well combined without obvious cavity and penetrating crack, coating with C/C matrices of composite materials, tensile strength
10.8MPa。
Embodiment two：
1) it is ρ=1.70g/cm by density by 30 × 10mm of φ specifications3C/C composite processing into sample, with 80
The polishing of mesh coarse sandpaper is allowed to surface roughening, is dried after cleaning；
2) Si powder, C powder, Al are bought with market2O3Powder is that raw material presses 5:1:0.5 ratio mixing, then puts mixed-powder
0.5h is stirred in ball blending machine, embedding powder is used as.Step 1 gained C/C samples are put into graphite crucible, and are embedded to above-mentioned powder
Material.Crucible is put into high-temperature vacuum graphitizing furnace under argon atmosphere, 1800 DEG C of insulation 2h must can have certain thickness
The C/C composite samples of SiC/Si coatings.Then make coating surface smooth with sand paper polishing, be cleaned and dried；
3) Si powder, W powder are bought with market, C powder is that raw material presses 6:6:1 ratio mixing, is then placed in ball by mixed-powder
0.5h is stirred in type mixer, embedding powder is used as.The C/C samples for there are SiC/Si coatings obtained by step 2 are put into graphite crucible, and
It is embedded to above-mentioned powder.Crucible is put into high-temperature vacuum graphitizing furnace under argon atmosphere, 2200 DEG C of insulation 2h can must have one
Determine the SiC/WSi of thickness2The C/C composite samples of coating.Then make coating surface smooth with sand paper polishing, be cleaned and dried；
4) PVA and water are pressed 1:7 ratio dissolves to be well mixed in 100 DEG C of constant water bath box is configured to PVA glues, will
Market is bought metal W powder and is mixed into wherein, and uniform suspension is formed after ultrasonic disperse 30min.Using LGZ-5 sponging granulators to original
Powder carries out granulation processing, obtains diameter 40um or so ball-type W spraying powders；
5) HEPJ type Supersonic Plasma Spraying equipment is used, is there is SiC/WSi2The C/C composite samples of transition zone
Surface is with power 55KW, powder sending quantity 4.0r/min, is prepared under primary air amount 77.4L/min spray parameters outside 50um or so W
Coating；
Prepared SiC-SiC/WSi of the invention2Transition zone and W external coatings are comparatively dense, and external coating voidage≤
2%, coating surface is well combined without obvious cavity and penetrating crack, coating with C/C matrices of composite materials, tensile strength
15.3MPa。
Embodiment three：
1) it is ρ=1.70g/cm by density by 10 × 10 × 10mm specifications3C/C composite processing into sample, use
The polishing of 80 mesh coarse sandpapers is allowed to surface roughening, is dried after cleaning；
2) Si powder, C powder, Al are bought with market2O3Powder is that raw material presses 5:1:0.5 ratio mixing, then puts mixed-powder
0.5h is stirred in ball blending machine, embedding powder is used as.Step 1 gained C/C samples are put into graphite crucible, and are embedded to above-mentioned powder
Material.Crucible is put into high-temperature vacuum graphitizing furnace under argon atmosphere, 2000 DEG C of insulation 2h must can have certain thickness
The C/C composite samples of SiC/Si coatings.Then make coating surface smooth with sand paper polishing, be cleaned and dried；
3) Si powder, W powder are bought with market, C powder is that raw material presses 6:5:1 ratio mixing, is then placed in ball by mixed-powder
0.5h is stirred in type mixer, embedding powder is used as.The C/C samples for there are SiC/Si coatings obtained by step 2 are put into graphite crucible, and
It is embedded to above-mentioned powder.Crucible is put into high-temperature vacuum graphitizing furnace under argon atmosphere, 2200 DEG C of insulation 2h can must have one
Determine the SiC/WSi of thickness2The C/C composite samples of coating.Then make coating surface smooth with sand paper polishing, be cleaned and dried；
4) PVA and water are pressed 1:7 ratio dissolves to be well mixed in 100 DEG C of constant water bath box is configured to PVA glues, will
Market is bought metal W powder and is mixed into wherein, and uniform suspension is formed after ultrasonic disperse 30min.Using LGZ-5 sponging granulators to original
Powder carries out granulation processing, obtains diameter 40um or so ball-type W spraying powders；
5) HEPJ type Supersonic Plasma Spraying equipment is used, is there is SiC/WSi2The C/C composite samples of transition zone
Surface is with power 55KW, powder sending quantity 4.0r/min, is prepared under primary air amount 77.4L/min spray parameters outside 50um or so W
Coating；
Prepared SiC/WSi of the invention2Transition zone and W external coatings are comparatively dense, external coating voidage≤2%, apply
Layer surface is well combined without obvious cavity and penetrating crack, coating with C/C matrices of composite materials, tensile strength 16.5MPa.
Claims (4)
1. a kind of preparation method of surface of carbon/carbon composite tungsten gradient coating, it is characterised in that step is as follows：
Step 1, pretreatment carbon/carbon compound material：Carbon/carbon compound material polishing is allowed to surface roughening, water is then used respectively
It is cleaned by ultrasonic with absolute ethyl alcohol, is placed in air and dries or oven for drying；
Step 2：By Si powder, C powder, Al2O3Powder is well mixed according to 65-80%, 10-25%, 5-15% mass ratio, is used as bag
Buried powder material is put into graphite crucible, step 1 is pre-processed in carbon/carbon compound material embedment powder, in carbon/carbon compound material table
Prepare SiC/Si transition zones in face；
Crucible is put into high-temperature vacuum graphitizing furnace under argon atmosphere, 1800~2000 DEG C of insulation 2h are had
The carbon/carbon compound material of SiC/Si coatings, then makes coating surface smooth, and be cleaned and dried with sand paper polishing；
Step 3：By 40-60% Si powder, 30-50% C powder, the mass ratio of 5-15% W powder is well mixed, and is used as embedding powder
Material is put into graphite crucible, and the carbon/carbon compound material with SiC/Si coatings that step 2 is obtained is embedded in powder；
Crucible is put into high-temperature vacuum graphitizing furnace under argon atmosphere, 2000~2200 DEG C of insulation 2h are had
SiC/WSi2The carbon/carbon compound material of transition zone, then makes coating surface smooth, and be cleaned and dried with sand paper polishing；
Step 4：PVA and water are pressed 1:7 ratio dissolves in 100 DEG C of constant water bath box is hybridly prepared into PVA glues, by metal
W powder is with PVA colloidal sols with 1:Uniform suspension is formed after 1 mass ratio mixing, ultrasonic disperse 30min, and carries out granulation processing, is obtained
Powder is sprayed to 30~50 μm of ball-type W of diameter；
Step 5：Using ball-type W powders as spraying powder, using HEPJ type Supersonic Plasma Spraying equipment in SiC/WSi2Undercoating
Surface of carbon/carbon composite W coatings, complete surface of carbon/carbon composite tungsten gradient coating preparation；The spraying
Technique is as follows：Spray power 50-60KW, primary air amount 70-80L/min, powder sending quantity 3.5-4.5r/min, nozzle tip to sample
Surface distance 10-13cm.
2. the preparation method of surface of carbon/carbon composite tungsten gradient coating according to claim 1, it is characterised in that：
The polishing of the step 1 uses 80 mesh coarse sandpapers.
3. the preparation method of surface of carbon/carbon composite tungsten gradient coating according to claim 1, it is characterised in that：
Being cleaned by ultrasonic with water and absolute ethyl alcohol for the step 1 is 5-10min.
4. the preparation method of surface of carbon/carbon composite tungsten gradient coating according to claim 1, it is characterised in that：
The granulation processing of the step 4 carries out granulation processing using LGZ-5 sponging granulators to powder.
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| CN106083217B (en) * | 2016-06-06 | 2018-12-28 | 西北工业大学 | The preparation method of surface of carbon/carbon composite reactive deposition metal W skeleton coating |
| CN106320876A (en) * | 2016-11-10 | 2017-01-11 | 无锡市明盛强力风机有限公司 | Sliding rail for automobile sliding door |
| CN108546156A (en) * | 2018-04-09 | 2018-09-18 | 西北工业大学 | The carbon/carbon compound material and preparation method that silicon carbide is modified with hydroxylapatite gradient coating |
| CN109852917B (en) * | 2019-01-31 | 2021-04-13 | 航天材料及工艺研究所 | Vacuum plasma spraying forming preparation method of molybdenum titanium zirconium member on surface of C/C, C/SiC composite material |
| CN111675552B (en) * | 2020-06-15 | 2022-02-11 | 江西宁新新材料股份有限公司 | High-temperature-resistant coating on graphite substrate and preparation method thereof |
| CN114105682B (en) * | 2021-11-26 | 2022-09-30 | 中钢热能金灿新能源科技(湖州)有限公司 | Improved method and device for prolonging service life of graphite crucible |
| CN115894082B (en) * | 2023-03-09 | 2023-06-23 | 中南大学 | (ZrHfTiTaNb) C-W metal high-entropy ceramic modified C/C composite material and preparation method thereof |
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| CN101293788A (en) * | 2008-06-26 | 2008-10-29 | 西北工业大学 | Method for preparing inoxidzable coating at high-temperature on carbon/carbon composite material surface |
| CN101863683B (en) * | 2009-04-15 | 2013-10-02 | 中国科学院上海硅酸盐研究所 | Anti-oxidation coating and preparation method thereof |
| CN101811892B (en) * | 2010-04-08 | 2012-07-04 | 西北工业大学 | Method for preparing nanowire-toughened carbon/carbon composite material ceramic coating |
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