CN101293788A - Method for preparing inoxidzable coating at high-temperature on carbon/carbon composite material surface - Google Patents
Method for preparing inoxidzable coating at high-temperature on carbon/carbon composite material surface Download PDFInfo
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- CN101293788A CN101293788A CNA2008101501420A CN200810150142A CN101293788A CN 101293788 A CN101293788 A CN 101293788A CN A2008101501420 A CNA2008101501420 A CN A2008101501420A CN 200810150142 A CN200810150142 A CN 200810150142A CN 101293788 A CN101293788 A CN 101293788A
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Abstract
The invention provides a preparation method of a high temperature oxidation-resistant coating on the surface of a carbon/carbon composite material. The preparation method comprises placing Si powder, C powder, and Al2O3 into an agate ball milling tank, adding distilled water, mixing and ball milling, taking out the mixed solution, and drying to form inner layer embedded powder; placing the treated C/C composite material into the powder in a graphite crucible; placing into a vertical type vacuum furnace with graphite being the heating body for preparing an undercoat; mixing the Si powder, Mo powder, W powder and C powder with absolute ethanol and silica sol to obtain slurry; and uniformly brush coating surface of the SiC inner layer of the C/C composite material I with the slurry, drying, and placing into an alumina crucible for preparing a top coating. The antioxidant protective time of the C/C composite material is increased from 100 hours in prior art to 200-252 hours in 1500 DEG C air using high temperature oxidation resistance of MoSi2 and WSi2 via combination of the undercoat and the top coating.
Description
Technical field
The present invention relates to a kind of preparation method of carbon/carbon compound material surface anti-oxidation coat.
Background technology
At carbon/carbon compound material surface preparation inoxidzable coating is the effective means that solves the easy problem of oxidation of carbon/carbon compound material.
Document 1 " Zhang Yulei; Li Hejun; Fu Qiangang.A Si-Mo oxidation protective coating for C/SiCcoated carbon/carbon composites.Carbon; 2007,45 (5): 1130-1133 " discloses a kind of slurry process and twice entrapping method of adopting respectively and has prepared the compound inoxidzable coating of C/SiC/Si-Mo at the C/C composite material surface.This coating is preparation method's complexity not only, and only can provide the C/C matrix material in 1500 ℃ of air and be no more than 100 hours protection against oxidation.
Document 2 " Multilayer coating with self-sealing properties for carbon-carbon composites; FedericoSmeacetto; Monica Ferraris; Milena Salvo; Carbon, 2003 41:2105-2111 " discloses a kind of employing slurry process with MoSi
2And Y
2O
3Particles dispersed has been alleviated the internal stress that does not match and cause owing to thermal expansivity in the coating in borosilicate glass, the coating of preparation has long-time anti-aging capability under 1300 ℃, but this coating does not possess high-temperature oxidation resistance.
Document 3 " Li Ke-Zhi, Hou Dang-She, Li He-Jun et al.Si-W-Mo coating for SiC coatedcarbon/carbon composites against oxidation.Surface ﹠amp; Coating Technology, 2007,201 (24): 9598-9602 " adopt twice entrapping method to prepare the SiC/Si-Mo-W compound coating at the C/C composite material surface, in 1500 ℃ of air, have long anti-aging capability.But this coating production is complicated, and the cycle is longer.In addition since the coating preparation temperature up to 2200 ℃～2400 ℃, this coatings applications when the C/C of the concrete complexity workpiece, is difficult in the coating avoid existing tiny crack, limited the real protection ability of coating.
Summary of the invention
In order to overcome short deficiency of prior art protection against oxidation time, the invention provides the preparation method of a kind of carbon/carbon compound material surface high-temperature oxidation resistant coating, the preparation method who adopts inside and outside layer to combine utilizes MoSi
2With WSi
2The excellent anti-oxidation performance of pyritous can improve carbon/carbon compound material surface high-temp antioxidizing guard time.
The technical solution adopted for the present invention to solve the technical problems:
The preparation method of a kind of carbon/carbon compound material surface high-temperature oxidation resistant coating is characterized in that comprising the steps:
(a) taking by weighing mass percent respectively is 65～80% Si powder, and mass percent is 5～20% C powder, and mass percent is 5～15% Al
2O
3Powder places agate jar, adds distilled water and carries out 10～15 hours ball milling combination treatment, mixed solution is taken out be dried into the first coating powder;
(b) will put into plumbago crucible through half of the embedding powder of step (a) preparation, put into C/C matrix material, put into second half investment covering again, add that then plumbago crucible covers through handling;
(c) plumbago crucible of adding a cover is put into the vertical vacuum furnace that graphite is made heating member, after vacuum oven vacuumized processing, with 5～10 ℃/min heat-up rate furnace temperature is risen to 1600～2000 ℃ from room temperature, be incubated 60～180 minutes, powered-down naturally cools to room temperature, and whole process is led to argon shield;
(d) taking by weighing mass percent respectively is 50～70% Si powder, mass percent is 15～25% Mo powder, mass percent is 10～20% W powder, mass percent is 1～5% C powder, adds dehydrated alcohol and silicon sol and is deployed into slip, carries out 10～20 minutes ultrasonic dispersing and handles, stir with magnetic stirring apparatus then, agitator speed is 2.5～3.5 revolutions per seconds, and churning time is 30～60 minutes, becomes outer slurry;
(e) slurry that step (d) is prepared is painted on the SiC internal layer surface through the C/C matrix material of step (c) preparation uniformly; put into alumina crucible after the oven dry; it is in 1450～1500 ℃ of high temperature box type resistance furnaces that crucible is inserted temperature; be incubated 20～60 minutes; powered-down naturally cools to room temperature, and whole process is led to argon shield.
The invention has the beneficial effects as follows: because the preparation method who adopts inside and outside layer to combine, with high purity Si powder, C powder, Al
2O
3Powder mixes by a certain percentage, and the C/C matrix material is embedded in this powder, at high temperature carries out sintering in protective atmosphere, obtains fine and close SiC undercoat.Skin is with being raw material with highly purified Si powder, Mo powder, W powder, C powder, is solvent with the dehydrated alcohol, mixes and is made into slip, with hairbrush this slip brushing is being had the C/C composite material surface of SiC internal layer, and high temperature sintering obtains (Mo in protective atmosphere
xW
1-x) Si
2-Si-SiC coating.Utilize MoSi
2With WSi
2Excellent high-temp antioxidizing performance makes in 1500 ℃ of air protection against oxidation time to the C/C matrix material bring up to 200～252 hours by prior art less than 100 hours.
Below in conjunction with drawings and Examples the present invention is elaborated.
Description of drawings
Fig. 1 is the inventive method embodiment 1 prepared (Mo
xW
1-x) Si
2The outer stereoscan photograph of-Si-SiC.
(the Mo that Fig. 2 the inventive method embodiment 1 is prepared
xW
1-x) Si
2The outer X ray diffracting spectrum of-Si-SiC.
Fig. 3 is the section backscattered electron photo of the inventive method embodiment 2 prepared coatings.
Fig. 4 is the inventive method embodiment 3 prepared coating samples isothermal oxidation weight loss curves in 1500 ℃ of air.
Embodiment
Embodiment 1: take by weighing the Si powder of 19g respectively, the C powder of 4g, the Al of 2g
2O
3Powder places agate jar, adds distilled water as the ball milling agent, carries out the ball milling combination treatment on planetary ball mill.Mixed powder: distilled water: agate ball=1: 3: 0.8, described ratio are mass ratio.Behind the ball milling 10 hours, mixed solution is taken out in 100 ℃ of oven dry down, the powder after the oven dry grinds and disperses the back standby as the embedding powder.Simultaneously the C/C matrix material is put into the ultrasonic wave washes clean with dehydrated alcohol behind the sanding and polishing successively with the sand paper of No. 400, No. 800 and No. 1000 respectively, in 100 ℃ of baking ovens, dry.The purity of Si powder is 99.5%, granularity is 400 orders, and the purity of C powder is 99%, granularity is 400 orders, Al
2O
3The purity of powder is 99.9%, granularity is 300 orders.The size and the quantity of agate ball are seen attached list.
Subordinate list: the diameter of agate ball and quantity
Half of the investment of above-mentioned steps preparation put into plumbago crucible, put into the C/C matrix material, put into second half investment again and cover, jiggle crucible then, make the even embedding C/C of investment matrix material, add crucible cover then.Whether plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member, vacuumize after 1 hour vacuum tightness is reached-0.09MPa, left standstill 1 hour, and observe vacuum meter and change, as no change, the illustrative system sealing is intact.With 10 ℃/min heat-up rate furnace temperature is risen to 2000 ℃ from room temperature, be incubated 1 hour, powered-down naturally cools to room temperature, and whole process is led to argon shield.Open crucible after the blow-on, from powder, take out the C/C matrix material, can see at material surface having one deck product to be the SiC internal layer after cleaning up.
Take by weighing the Si powder of 0.63g respectively, 0.19g the Mo powder, 0.15g the W powder, 0.03g the C powder, the powder of above-mentioned weighing is poured in the container that fills ethanolic soln, added minor amount of silicon colloidal sol again and carry out ultrasonic dispersing processing 10 minutes, utilize magnetic stirring apparatus to mix and make slip, agitator speed is 3 revolutions per seconds, and churning time is 30 minutes.Prepared pulp is painted on equably the C/C composite material surface that has the SiC internal layer; in 100 ℃ of baking ovens, put into alumina crucible after the oven dry; and crucible put into the good tubular type high temperature box type resistance furnace that heats up; design temperature is 1450 ℃; be incubated 30 minutes; powered-down naturally cools to room temperature, and whole process is led to argon shield.
From Fig. 1 stereoscan photograph and Fig. 2 X-Ray diffracting spectrum analysis revealed, the prepared skin of present embodiment is the (Mo of compact structure
xW
1-x) Si
2-Si-SiC (0＜x＜1) coating.
After testing, there is not the oxidation weight loss phenomenon in the prepared this duplex coating long-time oxidation under 1500 ℃ of high temperature of present embodiment.The coating sample is 1500 ℃ of airborne oxidation test results show, increases weight 1.42% 1500 ℃ of oxidations after 200 hours, and oxidation weight loss does not take place coating.
Embodiment 2: take by weighing the Si powder of 20g respectively, the C powder of 3.75g, the Al of 1.25g
2O
3Powder places agate jar, adds distilled water as the ball milling agent, carries out the ball milling combination treatment on planetary ball mill.Mixed powder: distilled water: agate ball=1: 3: 0.8, described ratio are mass ratio.Behind the ball milling 15 hours, mixed solution is taken out in 100 ℃ of oven dry down, the powder after the oven dry grinds and disperses the back standby as the embedding powder.Simultaneously the C/C matrix material is put into the ultrasonic wave washes clean with dehydrated alcohol behind the sanding and polishing successively with the sand paper of No. 400, No. 800 and No. 1000 respectively, in 100 ℃ of baking ovens, dry.The purity of Si powder is 99.5%, granularity is 400 orders, and the purity of C powder is 99%, granularity is 400 orders, Al
2O
3The purity of powder is 99.9%, granularity is 300 orders.The size of agate ball and quantity are seen embodiment 1 subordinate list.
Half of the investment of above-mentioned steps preparation put into plumbago crucible, put into the C/C matrix material, put into second half investment again and cover, jiggle crucible then, make the even embedding C/C of investment matrix material, add crucible cover then.Whether plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member, vacuumize after 30 minutes vacuum tightness is reached-0.09MPa, left standstill 1 hour, and observe vacuum meter and change, as no change, the illustrative system sealing is intact.With 5 ℃/min heat-up rate furnace temperature is risen to 1600 ℃ from room temperature, be incubated 3 hours, powered-down naturally cools to room temperature, and whole process is led to argon shield.Open crucible after the blow-on, from powder, take out the C/C matrix material, can see at material surface having one deck product to be the SiC internal layer after cleaning up.
Taking by weighing mass percent respectively is the Si powder of 0.6g, 0.2g the Mo powder, 0.15g the W powder, 0.05g the C powder, the powder of above-mentioned weighing is poured in the container that fills ethanolic soln, added minor amount of silicon colloidal sol again and carry out ultrasonic dispersing processing 20 minutes, utilize magnetic stirring apparatus to mix and make slip, agitator speed is 2.5 revolutions per seconds, and churning time is 1 hour.Prepared pulp is painted on equably the C/C composite material surface that has the SiC internal layer; in 100 ℃ of baking ovens, put into alumina crucible after the oven dry; and crucible put into the good tubular type high temperature box type resistance furnace that heats up; design temperature is 1500 ℃; be incubated 20 minutes; powered-down naturally cools to room temperature, and whole process is led to argon shield.
From Fig. 3 backscattered electron photo analysis revealed, white phase (Mo in the present embodiment coatings prepared skin
xW
1-x) Si
2(0＜x＜1) is evenly distributed among the grey form and aspect Si, has formed the heterogeneous structure of external coating (EC).
After testing, there is not the oxidation weight loss phenomenon in the prepared this duplex coating long-time oxidation under 1500 ℃ of high temperature of present embodiment.The coating sample is 1500 ℃ of airborne oxidation test results show, increases weight 1.28% 1500 ℃ of oxidations after 225 hours, and oxidation weight loss does not take place coating.
Embodiment 3: taking by weighing mass percent respectively is the Si powder of 16.25g, the C powder of 5g, the Al of 3.75g
2O
3Powder places agate jar, adds distilled water as the ball milling agent, carries out the ball milling combination treatment on planetary ball mill.Mixed powder: distilled water: agate ball=1: 3: 0.8, described ratio are mass ratio.Behind the ball milling 10 hours, mixed solution is taken out in 100 ℃ of oven dry down, the powder after the oven dry grinds and disperses the back standby as the embedding powder.Simultaneously the C/C matrix material is put into the ultrasonic wave washes clean with dehydrated alcohol behind the sanding and polishing successively with the sand paper of No. 400, No. 800 and No. 1000 respectively, in 100 ℃ of baking ovens, dry.The purity of Si powder is 99.5%, granularity is 400 orders, and the purity of C powder is 99%, granularity is 400 orders, Al
2O
3The purity of powder is 99.9%, granularity is 300 orders.The size of agate ball and quantity are seen embodiment 1 subordinate list.
Half of the investment of above-mentioned steps preparation put into plumbago crucible, put into the C/C matrix material, put into second half investment again and cover, jiggle crucible then, make the even embedding C/C of investment matrix material, add crucible cover then.Whether plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member, vacuumize after 30 minutes vacuum tightness is reached-0.09MPa, left standstill 1 hour, and observe vacuum meter and change, as no change, the illustrative system sealing is intact.With 10 ℃/min heat-up rate furnace temperature is risen to 1800 ℃ from room temperature, be incubated 2 hours, powered-down naturally cools to room temperature, and whole process is led to argon shield.Open crucible after the blow-on, from powder, take out the C/C matrix material, can see at material surface having one deck product to be the SiC internal layer after cleaning up.
Taking by weighing mass percent respectively is the Si powder of 0.65g, 0.25g the Mo powder, 0.08g the W powder, 0.02g the C powder, the powder of above-mentioned weighing is poured in the container that fills ethanolic soln, added minor amount of silicon colloidal sol again and carry out ultrasonic dispersing processing 20 minutes, utilize magnetic stirring apparatus to mix and make slip, agitator speed is 3 revolutions per seconds, and churning time is 30 minutes.Prepared pulp is painted on equably the C/C composite material surface that has the SiC internal layer; in 100 ℃ of baking ovens, put into alumina crucible after the oven dry; and crucible put into the good tubular type high temperature box type resistance furnace that heats up; design temperature is 1400 ℃; be incubated 1 hour; powered-down naturally cools to room temperature, and whole process is led to argon shield.After testing, there is not the oxidation weight loss phenomenon in the long-time oxidation under 1500 ℃ of high temperature of this duplex coating.
After testing, there is not the oxidation weight loss phenomenon in the prepared this duplex coating long-time oxidation under 1500 ℃ of high temperature of present embodiment.Fig. 4 floating coat sample is 1500 ℃ of airborne oxidation test results show, increases weight 1.56% 1500 ℃ of oxidations after 252 hours, and oxidation weight loss does not take place coating.
Claims (1)
1, the preparation method of the surperficial high-temperature oxidation resistant coating of a kind of carbon/carbon compound material is characterized in that comprising the steps:
(a) taking by weighing mass percent respectively is 65～80% Si powder, and mass percent is 5～20% C powder, and mass percent is 5～15% Al
2O
3Powder places agate jar, adds distilled water and carries out 10～15 hours ball milling combination treatment, mixed solution is taken out be dried into the first coating powder;
(b) will put into plumbago crucible through half of the embedding powder of step (a) preparation, put into C/C matrix material, put into second half investment covering again, add that then plumbago crucible covers through handling;
(c) plumbago crucible of adding a cover is put into the vertical vacuum furnace that graphite is made heating member, after vacuum oven vacuumized processing, with 5～10 ℃/min heat-up rate furnace temperature is risen to 1600～2000 ℃ from room temperature, be incubated 60～180 minutes, powered-down naturally cools to room temperature, and whole process is led to argon shield;
(d) taking by weighing mass percent respectively is 50～70% Si powder, mass percent is 15～25% Mo powder, mass percent is 10～20% W powder, mass percent is 1～5% C powder, adds dehydrated alcohol and silicon sol and is deployed into slip, carries out 10～20 minutes ultrasonic dispersing and handles, stir with magnetic stirring apparatus then, agitator speed is 2.5～3.5 revolutions per seconds, and churning time is 30～60 minutes, becomes outer slurry;
(e) slurry that step (d) is prepared is painted on the SiC internal layer surface through the C/C matrix material of step (c) preparation uniformly; put into alumina crucible after the oven dry; it is in 1450～1500 ℃ of high temperature box type resistance furnaces that crucible is inserted temperature; be incubated 20～60 minutes; powered-down naturally cools to room temperature, and whole process is led to argon shield.
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