CN101555164B - Preparation method of surface coating for enhancing high-temperature oxidation resistance of silicon carbide foam ceramic - Google Patents
Preparation method of surface coating for enhancing high-temperature oxidation resistance of silicon carbide foam ceramic Download PDFInfo
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- CN101555164B CN101555164B CN2008100109846A CN200810010984A CN101555164B CN 101555164 B CN101555164 B CN 101555164B CN 2008100109846 A CN2008100109846 A CN 2008100109846A CN 200810010984 A CN200810010984 A CN 200810010984A CN 101555164 B CN101555164 B CN 101555164B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 239000006260 foam Substances 0.000 title claims abstract description 55
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 53
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 230000003647 oxidation Effects 0.000 title claims abstract description 48
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 48
- 238000000576 coating method Methods 0.000 title claims abstract description 19
- 239000011248 coating agent Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 230000002708 enhancing effect Effects 0.000 title abstract 2
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 23
- 238000004544 sputter deposition Methods 0.000 claims abstract description 17
- 150000002500 ions Chemical class 0.000 claims abstract description 8
- 230000001590 oxidative effect Effects 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 20
- 238000000151 deposition Methods 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 238000007747 plating Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 15
- 229910004298 SiO 2 Inorganic materials 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 239000006261 foam material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 2
- 230000006851 antioxidant defense Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000002633 protecting effect Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- -1 PZS Chemical compound 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a preparation method of a surface coating for enhancing the high-temperature oxidation resistance of a silicon carbide foam ceramic, which belongs to the field of foam ceramic materials and the surface modification thereof. The method comprises the following steps: 1. the preoxidation treatment is performed to the silicon carbide foam ceramic for 1-10 hours at the temperature of 700-1300 DEG C; 2. as for the silicon carbide foam ceramic processed in the step 1 in the inert atmosphere or under the vacuum, a layer of metal Al is sputtered on the surface of the foam ceramic in an ion sputtering film plating machine by using an Al metal target; and 3. the silicon carbide foam ceramic processed in the step 2 is placed for 10-24 hours at the normal temperature in the air atmosphere, then is oxidized for 1-20 hours in the oxidative atmosphere at the temperature of 500-1200 DEG C and then is introduced with Ar or N2 protective gas to be raised to 1200-1550 DEG C and then preserved for 0.5-2 hours. Since a layer of dense high-temperature oxidation resistance coating is disposed on the surface of the silicon carbide foam ceramic, the fully new method has the advantages of high efficiency and adaptability, economy and reliability.
Description
Technical field:
The present invention relates to foam ceramic material and material surface modifying field, specifically refer to a kind of preparation method of surface coating that is used to improve high-temperature oxidation resistance of silicon carbide foam ceramic.
Background technology:
Screen like and porous ceramic is a kind of ceramic foam with three-dimensional networks structure; More and more cause people's attention in recent years; Especially foam silicon carbide ceramics is (referring to one Chinese patent application; Application number: 03134039.3, denomination of invention: foam silicon carbon stupalith of a kind of high strength dense and preparation method thereof, publication number: CN1600742A).As a kind of new function material; Foam silicon carbide ceramics can have higher open pore rate; And the essence that has kept the SiC pottery to a certain extent is like good characteristics such as low density, high-ratio surface, high-permeability, good high-temperature stability and heat-shock resistance, high chemical stability, long usage life-spans.Such ceramic foam is used at first metal melt particularly in the filtration of high-meltiing alloy more; Along with going deep into to its research; Increasing function is developed; As also can be used as processing, gasoline and diesel motor exhaust cleaner, support of the catalyst, solid thermal interchanger, porous burner device, thermal protection system of high-temperature flue gas etc., it has a kind of potential function in addition, promptly is used to prepare the mutually network combined material of metal-based or non-metal base co-continuous.
But silit is a kind of non-oxide ceramic material, under high temperature, oxidizing condition, inevitably brings problem of oxidation, though the oxidation products of SiC, SiO
2Protective membrane can stop the further generation of oxidation, still, about 800～1140 ℃, SiO
2Volume change can take place because of phase transformation in film, thereby makes protective membrane defectives such as crackle occur, and it is loose that structure becomes, and the oxidation protection effect greatly descends; Under atmosphere such as active oxidation, protective oxide layer also can't form in addition; Owing to preparing method's difference, material density, purity are also inequality, SiO simultaneously
2Oxide film, these factors all cause the sic foam material to cause use properties to descend because of oxidation, influence work-ing life.
At present; Resistance to high temperature oxidation treatment process to thyrite is a lot; As in thyrite, mixing oxide components, promptly form silicate bonded carbofrax material, the bonding crystal boundary that reaches mutually of this kind method all is a silicate mutually; All can play the anti-oxidation protection effect, but because this combination of material certainly will cause the performance of carbofrax material can be very not high; Have is exactly to form oxide protective layer on the carbofrax material surface again; Like systems such as zircon English, mullite, spinel, PZS, aluminum oxide; Coating production has coating method, sol-gel method, CVD, plasma spraying etc., and research shows that these methods can both play the better protecting effect.But with regard to present document and patent research; What aforesaid method was directed against all is compact block, fiber, whisker or powder etc.; Antioxidant defense for the foam silicon carbide ceramics of three-dimensional communication does not also have relevant report; The resistance to high temperature oxidation surface protection technique of silicon carbide foam ceramic material of the present invention proposes just in this case, should have very much development prospect.
Summary of the invention:
To the technological less present situation of improving the aspect at present about the foam silicon carbide ceramics high temperature oxidation resistance; The object of the invention just provides a kind of preparation method of surface coating that improves high-temperature oxidation resistance of silicon carbide foam ceramic; Form the fine and close resistance to high temperature oxidation coating of one deck on the foam silicon carbide ceramics surface, this kind new method has effectively, flexibility strong, the characteristics of economic and reliable.
Technical scheme of the present invention is:
Generally can in ceramic muscle surface and crystal boundary, form amorphous Si O after the foam silicon carbide ceramics oxidation
2Zone of oxidation, in the time of 800～1140 ℃, this unbodied SiO
2Can undergo phase transition, produce volume change, and then defective such as crack, the continuity of disruptive oxidation layer; Simultaneously, the impurity element in the material accumulates in the crystal boundary place more, destroys the SiO in the crystal boundary
2Can not form the bond structure of Si-O-Si, make oxygen in this zone of oxidation, to spread fast, two kinds of reasons all make the material oxidation rate quicken.
Based on top principle, the present invention proposes, and earlier with foam materials oxidation under certain condition, makes the surface form one deck SiO
2Zone of oxidation makes impurity element in the crystal boundary to surface diffusion, and to make this zone of oxidation be stable crystal form by no top form transformation, again at surface deposition Al, makes its oxidation form aluminum oxide, at high temperature handles then, and upper layer will form Al like this
2O
3-SiO
2The complex phase resist, thereby the high temperature oxidation resistance of foam materials is greatly enhanced.
The preparation method of surface coating of the raising high-temperature oxidation resistance of silicon carbide foam ceramic that the present invention proposes comprises the steps:
The first step, with foam silicon carbide ceramics 700～1300 ℃ of following pre-oxidation treatment 1～10 hour;
In second step, the foam silicon carbide ceramics of handling through the first step in the ion sputtering coating equipment, utilizes the Al metal targets, at foamed ceramics surface sputtering layer of metal Al under inert atmosphere or vacuum.
The 3rd step; The foam silicon carbide ceramics of handling through second step is in normal temperature air atmosphere held after 10～24 hours; Oxide treatment 1～20 hour (the preferred temperature of oxide treatment is 550-1000 ℃, and the preferred time is 5-10 hour) under 500～1200 ℃ of oxidizing atmospheres, and then feed Ar, N
2Be warming up to 1200～1550 ℃ of insulations 0.5～2 hour Deng shielding gas.
Specifically:
In the said the first step, the preoxidation condition is: air atmosphere, 700～1300 ℃ of following pre-oxidation treatment of temperature 1～10 hour form SiO on the surface
2Layer, thickness is 2～10 μ m.
In said second step, through foam silicon carbide ceramics surface sputtering one deck Al metal that the first step is handled, concrete steps are following:
(1) the Al metal targets is installed in the ion sputtering machine on the target platform;
(2) foam silicon carbide ceramics ultrasonic cleaning, the oven dry that will handle through the first step are installed in and can carry out on the continuous three-dimensional motion base material turntable;
(3) make the sputtering chamber vacuum be evacuated to (1～5) * 10
-3Pa perhaps vacuumizes the back and feeds inert atmosphere Ar gas or He gas etc.;
(4) power-on increases voltage gradually to build-up of luminance, and it is stabilized under the suitable power, keeps substrate bias suitable, and the base material three-dimensional motion is at foam silicon carbon ceramic surface deposition one deck Al film.Concrete processing parameter is: metallic target power is between 500～1500W, and substrate bias is between-100 to-400V; Sample can three-dimensional turn round, and the sample rotating speed is between 1～15rpm, and the depositing Al thickness of metal film is controlled between 1～50 μ m.
In said the 3rd step, the material behind the depositing Al layer is 20 hours in the normal temperature air atmosphere held time, and the temperature of oxide treatment is 1150 ℃, and the time is 5 hours, and the protective atmosphere treatment temp is 1350 ℃, and shielding gas is Ar or N
2Deng, soaking time is 1 hour.
The present invention has following advantage and effect:
What 1, the invention provides is a kind of brand-new antioxidant defense method that can be applied to the silicon carbide porous foam materials, and this method is simple to operate, cost is low, requires low to foam ceramic material.
2, flexibility of the present invention is strong, can use SiC foam ceramic material, the good reliability in multiple aperture, and after treatment stupalith oxidation resistance temperature and antioxidant property are all significantly improved.
Embodiment:
Embodiment 1:
The foam silicon carbide ceramics aperture of infiltration reaction sintering is 30PPi, consists of SiC, 13wt%Si and 2wt% impurity, and treating processes is:
(1) with foam silicon carbide ceramics 1300 ℃ of following pre-oxidation treatment 5 hours, form SiO on the foam silicon carbide ceramics surface
2Layer, present embodiment SiO
2Layer thickness is 10 μ m;
(2) foam silicon carbide ceramics of handling through step (1) in the vacuum ion sputtering coating equipment, utilizes the Al metal targets, and at foamed ceramics surface sputtering layer of metal Al, vacuum tightness is 1 * 10
-3Pa, metallic target power 1KW, substrate bias is at-200V, sample can the rotating speed 5rpm of three-dimensional running between, 20 minutes time, the depositing Al thickness of metal film is controlled at 4～8 μ m;
(3) through the foam silicon carbide ceramics that step (2) is handled was placed 10 hours in normal temperature air after, oxide treatment was 5 hours under 1150 ℃ of oxidizing atmospheres, and then fed N
2Be warming up to 1450 ℃ of insulations 1 hour as shielding gas.Finally, handle the oxidation resistance temperature that obtains material and can bring up to 1350 ℃, and the oxidation susceptibility under this temperature is not less than the oxidation susceptibility of material under 1000 ℃ that be untreated.
Embodiment 2:
The foam silicon carbide ceramics aperture of infiltration reaction sintering is 10PPi, consists of SiC, 15wt%Si and 3wt% impurity, and treating processes is:
(1) with foam silicon carbide ceramics 1200 ℃ of following pre-oxidation treatment 5 hours, form SiO on the foam silicon carbide ceramics surface
2Layer, present embodiment SiO
2Layer thickness is 6 μ m;
(2) foam silicon carbide ceramics of handling through step (1) in the vacuum ion sputtering coating equipment, utilizes the Al metal targets, at foamed ceramics surface sputtering layer of metal Al, vacuumizes (5 * 10
-3Pa) back feeds inert atmosphere Ar gas shiled, metallic target power 800W, substrate bias is at-300V, sample can the rotating speed 10rpm of three-dimensional running between, 60 minutes time, the depositing Al thickness of metal film is controlled at 30 μ m;
(3) through the foam silicon carbide ceramics that step (2) is handled was placed 15 hours in normal temperature air after, oxide treatment was 1 hour under 1200 ℃ of oxidizing atmospheres, and then fed Ar as protecting shielding gas to be warming up to 1400 ℃ of insulations 1.5 hours.Finally, handle the oxidation resistance temperature of the material that obtains and to bring up to 1300 ℃, and the oxidation susceptibility under this temperature is not less than the oxidation susceptibility of material under 1050 ℃ that be untreated.
Embodiment 3:
The foam silicon carbide ceramics aperture of infiltration reaction sintering is 5PPi, consists of SiC, 5wt%Si and 1wt% impurity, and treating processes is:
(1) with foam silicon carbide ceramics 1160 ℃ of following pre-oxidation treatment 2 hours, form SiO on the foam silicon carbide ceramics surface
2Layer, present embodiment SiO
2Layer thickness is 2 μ m;
(2) foam silicon carbide ceramics of handling through step (1) in the vacuum ion sputtering coating equipment, utilizes the Al metal targets, and at foamed ceramics surface sputtering layer of metal Al, vacuum tightness is 3 * 10
-3Pa, metallic target power 1400W, substrate bias is at-100V, sample can the rotating speed 8rpm of three-dimensional running between, 40 minutes time, the depositing Al thickness of metal film is controlled at 10 μ m;
(3) through the foam silicon carbide ceramics that step (2) is handled was placed 20 hours in normal temperature air after, oxide treatment was 20 hours under 500 ℃ of oxidizing atmospheres, and then fed N
2Be warming up to 1500 ℃ of insulations 1 hour as the protection shielding gas.Finally, handle the oxidation resistance temperature of the material that obtains and to bring up to 1400 ℃, and the oxidation susceptibility under this temperature is not less than the oxidation susceptibility of material under 1100 ℃ that be untreated.
Claims (4)
1. improve the preparation method of surface coating of high-temperature oxidation resistance of silicon carbide foam ceramic, it is characterized in that:
The first step, with foam silicon carbide ceramics 700～1300 ℃ of following pre-oxidation treatment 1～10 hour;
In second step, the foam silicon carbide ceramics of handling through the first step in the ion sputtering coating equipment, utilizes the Al metal targets, at foamed ceramics surface sputtering layer of metal Al under inert atmosphere or vacuum;
In the 3rd step, after 10～24 hours, oxide treatment is 1～20 hour under 500～1200 ℃ of oxidizing atmospheres, and then feeding Ar or N in normal temperature air atmosphere held for the foam silicon carbide ceramics of handling through second step
2Shielding gas is warming up to 1200～1550 ℃ of insulations 0.5～2 hour.
2. the preparation method of surface coating of raising high-temperature oxidation resistance of silicon carbide foam ceramic according to claim 1; It is characterized in that in the said the first step, the preoxidation condition is: air atmosphere; 700～1300 ℃ of following pre-oxidation treatment of temperature 1～10 hour form SiO on the surface
2Layer, thickness is 2～10 μ m.
3. the preparation method of surface coating of raising high-temperature oxidation resistance of silicon carbide foam ceramic according to claim 1 is characterized in that, in said second step, through foam silicon carbide ceramics surface sputtering one deck Al metal that the first step is handled, concrete steps are following:
(1) the Al metal targets is installed in the ion sputtering machine on the target platform;
(2) foam silicon carbide ceramics ultrasonic cleaning, the oven dry that will handle through the first step are installed in and can carry out on the continuous three-dimensional motion base material turntable;
(3) make the sputtering chamber vacuum be evacuated to 1～5 * 10
-3Pa perhaps vacuumizes the back and feeds inert atmosphere Ar gas or He gas;
(4) metallic target power is between 500～1500W, and substrate bias is between-100 to-400V, and the sample rotating speed is between 1～15rpm, and the depositing Al thickness of metal film is controlled between 1～50 μ m.
4. the preparation method of surface coating of raising high-temperature oxidation resistance of silicon carbide foam ceramic according to claim 1; It is characterized in that in said the 3rd step, the normal temperature air atmosphere held time is 20 hours; The temperature of oxide treatment is 1150 ℃, and the time is 5 hours; The protective atmosphere treatment temp is 1350 ℃, and shielding gas is Ar or N
2, soaking time is 1 hour.
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|---|---|---|---|
| CN2008100109846A CN101555164B (en) | 2008-04-11 | 2008-04-11 | Preparation method of surface coating for enhancing high-temperature oxidation resistance of silicon carbide foam ceramic |
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|---|---|---|---|
| CN2008100109846A CN101555164B (en) | 2008-04-11 | 2008-04-11 | Preparation method of surface coating for enhancing high-temperature oxidation resistance of silicon carbide foam ceramic |
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| CN101555164B true CN101555164B (en) | 2012-02-08 |
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| CN103722782B (en) * | 2013-09-11 | 2016-01-27 | 太仓派欧技术咨询服务有限公司 | A kind of ceramic matrix hybrid composite material and structure thereof |
| CN104876643B (en) * | 2015-05-11 | 2017-12-01 | 贵州大学 | Improve the surface treatment method of PTC-ceramic performance |
| CN105040407A (en) * | 2015-09-05 | 2015-11-11 | 苏州宏久航空防热材料科技有限公司 | Method for coating silicon carbide fiber surface with aluminum oxide coating |
| CN112299883B (en) * | 2019-07-26 | 2022-06-07 | 维沃泰克仪器(扬州)有限公司 | High-temperature-resistant protective coating of silicon carbide heating element and preparation method thereof |
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Non-Patent Citations (1)
| Title |
|---|
| 沈季雄.C/SiC复合材料表面SiC涂层的改性研究.《中国优秀博硕士学位论文全文数据库（硕士）工程科技I辑》.2004,(第3期),17. * |
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