CN101823900A - Method for forming silicide coating on surface of alumina-zirconia-carbon ceramic - Google Patents
Method for forming silicide coating on surface of alumina-zirconia-carbon ceramic Download PDFInfo
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- CN101823900A CN101823900A CN200910010565A CN200910010565A CN101823900A CN 101823900 A CN101823900 A CN 101823900A CN 200910010565 A CN200910010565 A CN 200910010565A CN 200910010565 A CN200910010565 A CN 200910010565A CN 101823900 A CN101823900 A CN 101823900A
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- China
- Prior art keywords
- carbon ceramic
- zirconia
- alumina
- zirconium
- coating
- Prior art date
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- 238000000576 coating method Methods 0.000 title claims abstract description 37
- 239000011248 coating agent Substances 0.000 title claims abstract description 36
- 229910021332 silicide Inorganic materials 0.000 title claims abstract description 23
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000000919 ceramic Substances 0.000 title claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 title abstract 7
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 13
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- -1 zirconium-aluminium-carbon Chemical compound 0.000 claims description 14
- 235000013312 flour Nutrition 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000009792 diffusion process Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 9
- 238000002156 mixing Methods 0.000 abstract description 6
- GJIKIPCNQLUSQC-UHFFFAOYSA-N bis($l^{2}-silanylidene)zirconium Chemical compound [Si]=[Zr]=[Si] GJIKIPCNQLUSQC-UHFFFAOYSA-N 0.000 abstract 1
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 230000017525 heat dissipation Effects 0.000 abstract 1
- 229910021353 zirconium disilicide Inorganic materials 0.000 abstract 1
- 229910006249 ZrSi Inorganic materials 0.000 description 9
- 230000003078 antioxidant effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229910003465 moissanite Inorganic materials 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 239000003963 antioxidant agent Substances 0.000 description 3
- 229910000851 Alloy steel Inorganic materials 0.000 description 2
- RQMIWLMVTCKXAQ-UHFFFAOYSA-N [AlH3].[C] Chemical compound [AlH3].[C] RQMIWLMVTCKXAQ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910000951 Aluminide Inorganic materials 0.000 description 1
- 229910008484 TiSi Inorganic materials 0.000 description 1
- 238000005269 aluminizing Methods 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
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Abstract
The invention relates to a method for forming a silicide coating on the surface of alumina-zirconia-carbon (Zr2Al3C4 and Zr3Al3C5) ceramic, belonging to the technical field of surface engineering. The method comprises the following steps that: solid powder mixture formed by silica powder and sodium fluoride powder in a mixing way is used as a permeable material, alumina-zirconia-carbon ceramic material is embedded in the permeable material, temperature is increased at a speed of 5-30 DEG C/min under the protection of inert gas, the temperature is kept to be 900-1300 DEG C for 0.5-5h, heat dissipation treatment is conducted, a furnace is cooled to room temperature and thereby a zirconium disilicide and silicon carbide coating is formed on the surface of a sample. Under the same oxidization conditions, the oxidation weight increase of the coating is decreased by 1-2 orders of magnitude when being compared with the oxidization weight increase of the alumina-zirconia-carbon ceramic material, thereby indicating that the oxidation resistance of the alumina-zirconia-carbon ceramic material can be greatly improved through a surface silica permeation method. The invention has the advantages that the use efficiency of the alumina-zirconia-carbon ceramic material is greatly improved, the application scope of the alumina-zirconia-carbon ceramic material is widened and the oxidation resistance of the coating is extremely high.
Description
Technical field
The invention belongs to surface engineering technology, specifically a kind of at zirconium aluminium carbon (Zr
2Al
3C
4And Zr
3Al
3C
5) ceramic surface forms the method for silicide coating.
Background technology
Zirconium aluminium carbon (Zr
2Al
3C
4And Zr
3Al
3C
5) stupalith is the ternary material of novel superhigh temperature resistant.They combine high-modulus, high rigidity, anti-oxidant, corrosion-resistant, high conductivity, high heat conductance, stronger advantages such as destruction tolerance.At high-technology fields such as Aeronautics and Astronautics, nuclear industry, ultrahigh-temperature structural parts the potential wide application prospect is arranged all.But as high-temperature structural material, their antioxidant property is not very desirable, has limited it in the high temperature oxidation stability environmental applications.Therefore, by surface modification, generating oxidation resistant protective coating is a kind of important channel of improving the structured material oxidation-resistance.For example, Liu etc. with the method for powder embedding siliconising at Ti
3SiC
2The surface generates a kind of TiSi
2/ SiC layer has improved Ti
3SiC
2High-temperature oxidation resistance reach two orders of magnitude (Mater.Res.Innnovations (investigation of materials innovation magazine) 6 (2002) 226).The method of usefulness pack aluminizings such as Xiang generates the antioxidant property (ActaMater. (material journal) 54 (2006) 4453) that aluminide coating has improved steel alloy on the steel alloy surface.But also there is not the zirconium-aluminium-carbon ceramic surface modification to improve the report of its oxidation-resistance aspect at present.
Summary of the invention
The object of the present invention is to provide a kind of method that forms silicide coating on the zirconium-aluminium-carbon ceramic surface, its technology is simple, with low cost, practical, particularly can improve the oxidation-resistance of zirconium-aluminium-carbon ceramic effectively.
To achieve these goals, technical scheme of the present invention is:
A kind of method that forms silicide coating on the zirconium-aluminium-carbon ceramic surface, the solid powder mixture that mixes with silica flour (Si) and Sodium Fluoride (NaF) is a bleed, the zirconium-aluminium-carbon ceramic material is put into bleed, under protection of inert gas, (be preferably 10～20 ℃/min) heat-up rate and be heated to 900～1300 ℃ (being preferably 1000～1200 ℃) with 5～30 ℃/min, be incubated 0.5～5 hour (being preferably 1～2 hour), stove is chilled to room temperature then; Through above-mentioned heat diffusion treatment, sample surfaces can form zirconium disilicide-silicon carbide (ZrSi of 2～150 micron thickness
2-SiC) coating, SiC and ZrSi
2Two-phase uniform mixing in coating distributes.
By weight percentage, composition consists of in the powdered mixture of the present invention: silica flour 95～99%, Sodium Fluoride 1～5%; Described silica flour purity 〉=99.00wt%, granularity≤0.2 millimeter; Sodium Fluoride is an analytical pure; Described rare gas element is the argon gas of bulk purity 〉=99%.
The present invention has following advantage:
1. adopt coatings prepared of the present invention to have high bonding strength and good antioxidant property.
2. the embedding raw material powder of the present invention's employing is simple, is silica flour and Sodium Fluoride powder.
3. to prepare silicide coating technology simple in the present invention, with the mixture embedding zirconium-aluminium-carbon ceramic sample of silica flour and Sodium Fluoride powder, through the elevated temperature heat diffusion, obtains silicide coating.Preparation process need not apply external force, need not carry out in a vacuum, and with low cost.
4. adopt the present invention can handle smooth surface, can also handle practical work piece with complex surface, practical.
5. because the present invention has utilized ZrSi
2With the antioxidant property of the excellence of SiC, will improve the range of application of zirconium-aluminium-carbon ceramic material greatly so use the present invention.
Description of drawings
Fig. 1 is Zr of the present invention
3Al
3C
5Ooze the silicide coating stereoscan photograph that Si handles rear surface formation in 2 hours through 1200 ℃.
Fig. 2 is Zr of the present invention
2Al
3C
4Ooze the silicide coating stereoscan photograph that Si handles rear surface formation in 1 hour through differing temps.(a)1000℃；(b)1100℃；(c)1200℃。Among the figure, Resin represents resin; Scale represents silicide layer, by ZrSi
2Form with SiC; Substrate represents Zr
2Al
3C
4Matrix.
Fig. 3 is for comparing Zr
2Al
3C
4Through oozing the sample and the Zr that does not ooze Si after Si handles
2Al
3C
4The oxidation weight gain curve of sample; Among the figure, cementedZr
2Al
3C
4The sample behind the Si is oozed in representative.
Embodiment
Below in conjunction with drawings and Examples in detail the present invention is described in detail.
Embodiment 1
The composition of solid powder mixture of the present invention: silica flour purity 〉=99.00wt%, granularity≤0.2 millimeter; Sodium Fluoride is an analytical pure.
The concrete data of present embodiment are: Zr
3Al
3C
5Sample size is 10mm * 4mm * 4mm, and powdered mixture is formed by weight percentage: 99% silicon, 1% Sodium Fluoride, gross weight are 5g.Take out system vacuum to 10Pa, charge into argon gas (99.99%Ar) then, Heating temperature is 1200 ℃, and heat-up rate is 15 ℃/min, and soaking time is 2 hours, and stove takes out sample after being chilled to room temperature.Accompanying drawing 1 is seen in the silicide coating cross section that generates.Black is SiC in the coating, and grey is ZrSi
2, SiC and ZrSi
2Two-phase uniform mixing in coating distributes.Coat-thickness is about 60 microns.
Embodiment 2
Difference from Example 1 is:
Zr
2Al
3C
4Material sample 10mm * 4mm * 4mm, powdered mixture is formed by weight percentage: 98% silicon, 2% Sodium Fluoride, gross weight are 8g; Heating temperature is 1000 ℃, and heat-up rate is 10 ℃/min, and soaking time is 1 hour, and stove takes out sample after being chilled to room temperature.Accompanying drawing 2 (a), SiC and ZrSi are seen in the silicide coating cross section that generates
2Two-phase uniform mixing in coating distributes, and coat-thickness is about 12 microns.
Difference from Example 1 is:
Zr
2Al
3C
4Material sample 8mm * 5mm * 5mm, powdered mixture is formed by weight percentage: 97% silicon, 3% Sodium Fluoride, gross weight are 7g; Heating temperature is 1100 ℃, and heat-up rate is 20 ℃/min, and soaking time is 1 hour, and stove takes out sample after being chilled to room temperature.Accompanying drawing 2 (b), SiC and ZrSi are seen in the silicide coating cross section that generates
2Two-phase uniform mixing in coating distributes, and coat-thickness is about 40 microns.
Difference from Example 1 is:
Zr
2Al
3C
4Material sample 6mm * 6mm * 5mm, powdered mixture is formed by weight percentage: 96% silicon, 4% Sodium Fluoride, gross weight are 6g; Heating temperature is 1200 ℃, and heat-up rate is 15 ℃/min, and soaking time is 1 hour, and stove takes out sample after being chilled to room temperature.Accompanying drawing 2 (c), SiC and ZrSi are seen in the silicide coating cross section that generates
2Two-phase uniform mixing in coating distributes, and coat-thickness is about 53 microns.
Comparative example
By non-constant temperature oxidation control experiment, see accompanying drawing 3 (a) as can be known, adopt the Zr that contains silicide coating with embodiment 4 prepared
2Al
3C
4Weightening finish than the Zr that does not contain coating
2Al
3C
4Much lower, particularly more than 1100 ℃.By the constant temperature oxidation control experiment, see accompanying drawing 3 (b) as can be known, adopt the Zr that contains silicide coating with embodiment 2-4 prepared
2Al
3C
4Weightening finish than the Zr that does not contain coating
2Al
3C
4Hang down 1-2 the order of magnitude.This shows, contain the Zr of silicide coating
2Al
3C
4Antioxidant property than the Zr that does not contain coating
2Al
3C
4Antioxidant property huge improvement has been arranged.
Claims (5)
1. method that forms silicide coating on zirconium-aluminium-carbon ceramic surface; it is characterized in that: the solid powder mixture that mixes with silica flour and Sodium Fluoride powder is a bleed; the zirconium-aluminium-carbon ceramic material is embedded in the bleed; under protection of inert gas; with the heat-up rate of 5～30 ℃/min, under 900～1300 ℃ of conditions, the insulation 0.5～5 hour; carry out heat diffusion treatment, stove is chilled to room temperature then, promptly forms with zirconium disilicide-coat of silicon carbide at sample surfaces.
2. according to the described method that forms silicide coating on zirconium-aluminium-carbon ceramic surface of claim 1, it is characterized in that: percentage meter by weight, the consisting of of described powdered mixture: silica flour 95～99%, Sodium Fluoride 1～5%.
3. according to the described method that forms silicide coating on the zirconium-aluminium-carbon ceramic surface of claim 1, it is characterized in that: the thickness of zirconium disilicide-coat of silicon carbide is 2～150 microns.
4. according to the described method that forms silicide coating on zirconium-aluminium-carbon ceramic surface of claim 1, it is characterized in that: described silica flour purity 〉=99.00wt%, granularity≤0.2 millimeter; Sodium Fluoride is an analytical pure.
5. according to the described method that forms silicide coating on the zirconium-aluminium-carbon ceramic surface of claim 1, it is characterized in that: described rare gas element is the argon gas of purity 〉=99.99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910010565A CN101823900A (en) | 2009-03-04 | 2009-03-04 | Method for forming silicide coating on surface of alumina-zirconia-carbon ceramic |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910010565A CN101823900A (en) | 2009-03-04 | 2009-03-04 | Method for forming silicide coating on surface of alumina-zirconia-carbon ceramic |
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|---|---|
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104928742A (en) * | 2015-06-12 | 2015-09-23 | 中国科学院金属研究所 | MAX phase ceramic and composite material surface modification processing method thereof |
| CN107056303A (en) * | 2017-04-14 | 2017-08-18 | 河南工业大学 | It is a kind of to prepare ZrB in zirconium aluminium carbon/carbon/silicon carbide composite material surface2The method of/SiC coatings |
-
2009
- 2009-03-04 CN CN200910010565A patent/CN101823900A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104928742A (en) * | 2015-06-12 | 2015-09-23 | 中国科学院金属研究所 | MAX phase ceramic and composite material surface modification processing method thereof |
| CN104928742B (en) * | 2015-06-12 | 2017-08-11 | 中国科学院金属研究所 | The processing method that a kind of MAX phase ceramics and its composite material surface are modified |
| CN107056303A (en) * | 2017-04-14 | 2017-08-18 | 河南工业大学 | It is a kind of to prepare ZrB in zirconium aluminium carbon/carbon/silicon carbide composite material surface2The method of/SiC coatings |
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Application publication date: 20100908 |