CN101811892B - Method for preparing nanowire-toughened carbon/carbon composite material ceramic coating - Google Patents
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Abstract
The invention discloses a method for preparing a nanowire-toughened carbon/carbon composite material ceramic coating. The method aims to solve the technical problem that the ceramic coating prepared by a conventional method has poor denseness. The method adopts the following technical scheme that: the nanowire-toughened carborundum (SiC)-molybdenum disilicide (MoSi2)-chromium silicide (CrSi2) ceramic coating is prepared by chemical vapor deposition, the cracking trend of the coating is reduced, and the ceramic coating with a dense structure is prepared by means of the toughening effect of nanowires. The effective anti-oxidization time of the prepared ceramic coating in atmosphere at the temperature of 1,500 DEG C is improved to 140 and 155 hours from 50 hours in background technology.
Description
Technical field
The present invention relates to the preparation method of a kind of preparation method of carbon/carbon compound material ceramic coating, particularly nanowire-toughened carbon/carbon/carbon composite (hereinafter to be referred as the C/C matrix material) ceramic coating.
Background technology
It is the most difficult bottleneck problem that breaks through in the actual application of heat structure C/C matrix material that high temperature is prone to oxidation; The investigator has proposed many solutions both at home and abroad; And be a kind of effective means at its surface preparation inoxidzable coating; Wherein, ceramic coating have good antioxidant property and with C/C matrix material better physical chemical compatibility, be C/C matrix material ideal coated material.Yet the fragility of ceramic coating is its most difficult bottleneck of breaking through in actual application.The major cause of the anti-oxidation inefficacy of existing ceramic coating system is the mismatch in coefficient of thermal expansion because of ceramic coating and C/C matrix; Make the bigger thermal stresses of existence in the ceramic coating; Cause ceramic coating easy to crack in high low temperature alternation process; In order to have alleviated the cracking trend of ceramic coating, crystal whisker toughened ceramic coating technology has caused researchist's very big concern.
Document " A SiC whisker-toughened SiC-CrSi
2Oxidation protective coating forcarbon/carbon composites; Fu Qiangang; Li Hejun, Shi Xiaohong, Li Kezhi; And Zhang Wei, Huang Min.Applied Surface Science 2007 (253): 3757-3760 " a kind of crystal whisker toughened SiC-CrSi of two steps technology preparation SiC that adopts slurry process and entrapping method to combine disclosed
2The method of ceramic coating, this method at first adopt slurry process to prepare the crystal whisker toughened SiC coating of porous SiC at the C/C composite material surface; Secondly, adopt entrapping method to make the Si-Cr alloy fill the hole in the crystal whisker toughened SiC coating of SiC.Although this technology has been alleviated the cracking trend of ceramic coating in high low temperature alternation process to a certain extent, the toughness reinforcing effect of crystal whisker toughened ceramic coating is undesirable.Because the SiC whisker be prone to be reunited in coating, disperse inhomogeneously, make toughening effect limited; And SiC whisker size is bigger; Can spread by the hinder coating powder, make coating fine and close inadequately, have big hole; Reduce the anti-oxidation performance of this coating greatly, as 1500 ℃ of oxidations after 50 hours coating test specimen rate of weight loss reached 0.66%.
Summary of the invention
For the deficiency of the ceramic coating compactness difference that overcomes existing method preparation, the present invention provides a kind of preparation method of nanowire-toughened C/C composite material ceramic coating.This method adopts chemical vapour deposition to prepare the nanowire-toughened SiC-MoSi of SiC
2-CrSi
2Ceramic coating by nanowire-toughened effect, can reduce the cracking trend of coating, prepares the ceramic coating of compact structure.
The technical solution adopted for the present invention to solve the technical problems: a kind of preparation method of nanowire-toughened C/C composite material ceramic coating is characterized in that comprising the steps:
1) with cleaning behind the C/C matrix material sanding and polishing, puts into baking oven and dry;
2) taking by weighing mass percent respectively is 10～20% Si powder, 15～30% C powder, 55～75% SiO
2Powder places the rosin ball grinder, and ball mill mixing was handled 2～4 hours;
3) with step 2) powder of preparation puts into plumbago crucible, and making its powder thickness is 1/5 of the plumbago crucible degree of depth, and the C/C matrix material of again step 1) being handled is suspended on the surperficial top of powder in the plumbago crucible after with the binding of charcoal fiber;
4) plumbago crucible is put into the vacuum reaction stove, vacuum oven is carried out vacuum-treat after, logical argon gas rises to 1600～1700 ℃ with furnace temperature from room temperature with 5～10 ℃/min heat-up rate to normal pressure, is incubated 1～3 hour; Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process;
5) taking by weighing mass percent respectively is 40～65% Si powder, 5～10% C powder, 20～30% MoSi
2Powder, 10～20% Cr powder places the rosin ball grinder, and ball mill mixing was handled 2～4 hours;
6) half puts into plumbago crucible with the powder of step 5) preparation, puts into the C/C matrix material that contains the SiC nano wire through the surface of step 4) preparation again, puts into the C/C matrix material that second half embedding powder contains the SiC nano wire with the surface subsequently and covers;
7) plumbago crucible is put into the vacuum reaction stove, vacuum oven is carried out vacuum-treat after, logical argon gas rises to 2100～2300 ℃ with furnace temperature from room temperature with 5～10 ℃/min heat-up rate to normal pressure, is incubated 1～3 hour; Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.
The invention has the beneficial effects as follows: owing to adopt chemical vapour deposition to prepare the nanowire-toughened SiC-MoSi of SiC
2-CrSi
2Ceramic coating by nanowire-toughened effect, has reduced the cracking trend of coating, prepares the ceramic coating of compact structure.Prepared ceramic coating is brought up to 140～155 hours 1500 ℃ of airborne effective anti-oxidization time by 50 hours of background technology.
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
Description of drawings
Fig. 1 is the prepared SiC nanowire surface stereoscan photograph of the embodiment of the invention 2.
Fig. 2 is the prepared nanowire-toughened ceramic coating surface scan of the SiC electromicroscopic photograph of the embodiment of the invention 2.
Fig. 3 is the prepared nanowire-toughened ceramic coating profile scanning of the SiC electromicroscopic photograph of the embodiment of the invention 2.
Fig. 4 is 1500 ℃ of oxidation weight loss curves of C/C matrix material that the embodiment of the invention 2 prepared surfaces contain the nanowire-toughened ceramic coating of SiC.
Embodiment
Embodiment 1: the sand paper that the C/C matrix material is used No. 400, No. 800 and No. 1000 respectively is clean with absolute ethanol washing behind the sanding and polishing successively, dry for standby in baking oven.
Take by weighing the Si powder of 10g respectively, the C powder of 25g and the SiO of 65g
2Powder.Place the rosin ball grinder, get the agate ball of different quantities different diameter and put into the rosin ball grinder, on planetary ball mill, carry out ball mill mixing and handle 2h, subsequent use as powder.
Powder is put into plumbago crucible, and making its powder thickness is 1/5th of the plumbago crucible degree of depth, is suspended on the top on powder surface after the C/C matrix material after will drying again bundlees with a branch of 3K charcoal fiber, then plumbago crucible is put into the vacuum reaction stove.Vacuumize after 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity is observed vacuum meter and is indicated whether to change, and like no change, the illustrative system sealing is intact.Logical argon gas is to normal pressure.This process triplicate.Afterwards furnace temperature is risen to 1600 ℃, temperature rise rate is 5 ℃/min, is incubated 2 hours then.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out plumbago crucible subsequently, the charcoal fiber on the cleaning C/C matrix material obtains the C/C matrix material that the SiC nano wire is contained on the surface.
Take by weighing the Si powder of 40g respectively, the C powder of 10g, the MoSi of 30g
2Powder, the Cr powder of 20g.Place the rosin ball grinder, get the agate ball of different quantities different diameter and put into the rosin ball grinder, on planetary ball mill, carry out ball mill mixing and handled 3 hours, subsequent use as investment.
Half of above-mentioned investment put into plumbago crucible; Put into the surface for preparing and contain the C/C matrix material of SiC nano wire; Put into second half investment again; The slight plumbago crucible that rocks makes investment contain the C/C matrix material of SiC nano wire in the embedding surface equably, then plumbago crucible is put into the vacuum reaction stove.Vacuumize after 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity is observed vacuum meter and is indicated whether to change, and like no change, the illustrative system sealing is intact.Logical argon gas is to normal pressure.This process triplicate.Afterwards furnace temperature is risen to 2100 ℃, temperature rise rate is 7 ℃/min, is incubated 2 hours then.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out plumbago crucible subsequently, cleaning embedding powder obtains containing the nanowire-toughened SiC-MoSi of SiC
2-CrSi
2The C/C matrix material of ceramic coating.
Oxidation experiment shows: the SiC-MoSi that SiC is nanowire-toughened
2-CrSi
2Ceramic coating reaches 140 hours 1500 ℃ of airborne effective anti-oxidization time.
Embodiment 2: the sand paper that the C/C matrix material is used No. 400, No. 800 and No. 1000 respectively is clean with absolute ethanol washing behind the sanding and polishing successively, dry for standby in baking oven.
Take by weighing the Si powder of 15g respectively, the C powder of 30g and the SiO of 75g
2Powder.Place the rosin ball grinder, get the agate ball of different quantities different diameter and put into the rosin ball grinder, on planetary ball mill, carry out ball mill mixing and handle 3h, subsequent use as powder.
Powder is put into plumbago crucible, and making its powder thickness is 1/5th of the plumbago crucible degree of depth, is suspended on the top on powder surface after the C/C matrix material after will drying by the fire again bundlees with a branch of 3K charcoal fiber, then plumbago crucible is put into the vacuum reaction stove.Vacuumize after 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity is observed vacuum meter and is indicated whether to change, and like no change, the illustrative system sealing is intact.Logical argon gas is to normal pressure.This process triplicate.Afterwards furnace temperature is risen to 1650 ℃, temperature rise rate is 7 ℃/min, is incubated 3 hours then.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out plumbago crucible subsequently, the charcoal fiber on the cleaning C/C matrix material obtains the C/C matrix material that the SiC nano wire is contained on the surface.
The Si powder of the 50g that takes by weighing respectively, the C powder of 8g, the MoSi of 27g
2Powder, the Cr powder of 15g.Place the rosin ball grinder, get the agate ball of different quantities different diameter and put into the rosin ball grinder, on planetary ball mill, carry out ball mill mixing and handled 4 hours, subsequent use as investment.
Half of above-mentioned investment put into plumbago crucible; Put into the surface for preparing and contain the C/C matrix material of SiC nano wire; Put into second half investment again; The slight plumbago crucible that rocks makes investment contain the C/C matrix material of SiC nano wire in the embedding surface equably, then plumbago crucible is put into the vacuum reaction stove.Vacuumize after 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity is observed vacuum meter and is indicated whether to change, and like no change, the illustrative system sealing is intact.Logical argon gas is to normal pressure.This process triplicate.Afterwards furnace temperature is risen to 2200 ℃, temperature rise rate is 10 ℃/min, is incubated 3 hours then.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out plumbago crucible subsequently, cleaning embedding powder obtains containing the nanowire-toughened SiC-MoSi of SiC
2-CrSi
2The C/C matrix material of ceramic coating.
Visible by Fig. 1, the SiC nano wire of the C/C composite material surface that chemical vapour deposition obtains is orientated random distribution, has formed loose vesicular structure.Visible by Fig. 2, the nanowire-toughened ceramic coating compact structure of the SiC of preparation does not have defectives such as obvious hole and crackle.Visible by Fig. 3, preparation the SiC nano wire in ceramic coating, be orientated in a jumble, be uniformly dispersed.Can know the nanowire-toughened SiC-MoSi of SiC by Fig. 4
2-CrSi
2The ceramic coating anti-aging capability obviously improves, and reaches 155 hours 1500 ℃ of airborne effective anti-oxidization time.
Embodiment 3: the sand paper that the C/C matrix material is used No. 400, No. 800 and No. 1000 respectively is clean with absolute ethanol washing behind the sanding and polishing successively, dry for standby in baking oven.
Take by weighing the Si powder of 20g respectively, the C powder of 15g and the SiO of 55g
2Powder.Place the rosin ball grinder, get the agate ball of different quantities different diameter and put into the rosin ball grinder, on planetary ball mill, carry out ball mill mixing and handle 4h, subsequent use as powder.
Powder is put into plumbago crucible, and making its powder thickness is 1/5th of the plumbago crucible degree of depth, is suspended on the top on powder surface after the C/C matrix material after will drying by the fire again bundlees with a branch of 3K charcoal fiber, then plumbago crucible is put into the vacuum reaction stove.Vacuumize after 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity is observed vacuum meter and is indicated whether to change, and like no change, the illustrative system sealing is intact.Logical argon gas is to normal pressure.This process triplicate.Afterwards furnace temperature is risen to 1700 ℃, temperature rise rate is 10 ℃/min, is incubated 1 hour then.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out plumbago crucible subsequently, the charcoal fiber on the cleaning C/C matrix material obtains the C/C matrix material that the SiC nano wire is contained on the surface.
The Si powder of the 65g that takes by weighing respectively, the C powder of 5g, the MoSi of 20g
2Powder, the Cr powder of 10g.Place the rosin ball grinder, get the agate ball of different quantities different diameter and put into the rosin ball grinder, on planetary ball mill, carry out ball mill mixing and handled 2 hours, subsequent use as investment.
Half of above-mentioned investment put into plumbago crucible; Put into the surface for preparing and contain the C/C matrix material of SiC nano wire; Put into second half investment again; The slight plumbago crucible that rocks makes investment contain the C/C matrix material of SiC nano wire in the embedding surface equably, then plumbago crucible is put into the vacuum reaction stove.Vacuumize after 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity is observed vacuum meter and is indicated whether to change, and like no change, the illustrative system sealing is intact.Logical argon gas is to normal pressure.This process triplicate.Afterwards furnace temperature is risen to 2300 ℃, temperature rise rate is 5 ℃/min, is incubated 1 hour then.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out plumbago crucible subsequently, cleaning embedding powder obtains containing the nanowire-toughened SiC-MoSi of SiC
2-CrSi
2The C/C matrix material of ceramic coating.
Oxidation experiment shows: the SiC-MoSi that SiC is nanowire-toughened
2-CrSi
2Ceramic coating reaches 150 hours 1500 ℃ of airborne effective anti-oxidization time.
Among all embodiment, the purity of Si powder is 99.5%, granularity is 300 orders, and the purity of C powder is 99%, granularity is 320 orders, SiO
2The purity check of powder is pure, granularity is 300 orders, MoSi
2The purity of powder is 99%, granularity is 300 orders, and the purity of Cr powder is that high-purity, granularity is 200 orders.
Claims (1)
1. the preparation method of a nanowire-toughened carbon/carbon/carbon/carbon composite material ceramic coating is characterized in that comprising the steps:
1) with cleaning behind the C/C matrix material sanding and polishing, puts into baking oven and dry;
2) taking by weighing mass percent respectively is 10～20% Si powder, 15～30% C powder, 55～75% SiO
2Powder places the rosin ball grinder, and ball mill mixing was handled 2～4 hours;
3) with step 2) powder of preparation puts into plumbago crucible, and making its powder thickness is 1/5 of the plumbago crucible degree of depth, and the C/C matrix material of again step 1) being handled is suspended on the surperficial top of powder in the plumbago crucible after with the binding of charcoal fiber;
4) plumbago crucible is put into the vacuum reaction stove, vacuum oven is carried out vacuum-treat after, logical argon gas rises to 1600～1700 ℃ with furnace temperature from room temperature with 5～10 ℃/min heat-up rate to normal pressure, is incubated 1～3 hour; Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process;
5) taking by weighing mass percent respectively is 40～65% Si powder, 5～10% C powder, 20～30% MoSi
2Powder, 10～20% Cr powder places the rosin ball grinder, and ball mill mixing was handled 2～4 hours;
6) half puts into plumbago crucible with the powder of step 5) preparation, puts into the C/C matrix material that contains the SiC nano wire through the surface of step 4) preparation again, puts into the C/C matrix material that second half embedding powder contains the SiC nano wire with the surface subsequently and covers;
7) plumbago crucible is put into the vacuum reaction stove, vacuum oven is carried out vacuum-treat after, logical argon gas rises to 2100～2300 ℃ with furnace temperature from room temperature with 5～10 ℃/min heat-up rate to normal pressure, is incubated 1～3 hour; Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214268A (en) * | 2013-03-28 | 2013-07-24 | 西北工业大学 | Preparation method of nano-wire reinforced SiC wear-resistant coating |
| CN103214268B (en) * | 2013-03-28 | 2014-10-29 | 西北工业大学 | Preparation method of nano-wire reinforced SiC wear-resistant coating |
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