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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- Prior art keywords
- zirconium
- coating
- aluminum carbon
- carbon ceramic
- silicide coating
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- 238000000576 coating method Methods 0.000 title claims abstract description 39
- 239000011248 coating agent Substances 0.000 title claims abstract description 38
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 title 1
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 25
- -1 zirconium aluminum carbon Chemical compound 0.000 claims abstract description 19
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 12
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 6
- 238000009792 diffusion process Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract 4
- 239000011863 silicon-based powder Substances 0.000 claims abstract 4
- 238000004321 preservation Methods 0.000 claims abstract 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 230000008595 infiltration Effects 0.000 claims 1
- 238000001764 infiltration Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 150000003385 sodium Chemical class 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 10
- 238000007254 oxidation reaction Methods 0.000 abstract description 10
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 6
- 230000004584 weight gain Effects 0.000 abstract description 2
- 235000019786 weight gain Nutrition 0.000 abstract description 2
- 238000005475 siliconizing Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 229910006249 ZrSi Inorganic materials 0.000 description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 9
- 235000013312 flour Nutrition 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 230000003078 antioxidant effect Effects 0.000 description 5
- 229910003465 moissanite Inorganic materials 0.000 description 5
- 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
- 239000007789 gas 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
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Abstract
本发明属于表面工程技术，具体地说是一种在锆铝碳(Zr2Al3C4和Zr3Al3C5)陶瓷表面形成硅化物涂层的方法。该方法用硅粉和氟化钠粉混合而成的固体粉末混合物为渗料，将锆铝碳陶瓷材料包埋在渗料中，在惰性气体保护下，以5～30℃/min的升温速度、在900～1300℃条件下、保温0.5～5小时，进行热扩散处理，然后炉冷至室温，即在样品表面形成以二硅化锆-碳化硅涂层。相同氧化条件下涂层的氧化增重比锆铝碳陶瓷材料氧化增重降低了1-2个数量级，表明通过表面渗硅的方法可以极大地提高锆铝碳陶瓷材料的抗氧化性能。本发明将大大提高锆铝碳陶瓷材料的使用效率并拓宽其应用范围，使涂层具有极高的抗氧化性能。The invention belongs to surface engineering technology, in particular to a method for forming a silicide coating on the surface of zirconium aluminum carbon (Zr 2 Al 3 C 4 and Zr 3 Al 3 C 5 ) ceramics. In this method, the solid powder mixture formed by mixing silicon powder and sodium fluoride powder is used as the infiltrating material, and the zirconium-aluminum carbon ceramic material is embedded in the infiltrating material. 1. Under the condition of 900-1300 ℃, heat preservation for 0.5-5 hours, carry out thermal diffusion treatment, and then furnace cool to room temperature, that is to form a zirconium disilicide-silicon carbide coating on the surface of the sample. Under the same oxidation conditions, the oxidation weight gain of the coating is 1-2 orders of magnitude lower than that of the zirconium aluminum carbon ceramic material, indicating that the oxidation resistance of the zirconium aluminum carbon ceramic material can be greatly improved by surface siliconizing. The invention will greatly improve the use efficiency of the zirconium aluminum carbon ceramic material and broaden its application range, so that the coating has extremely high oxidation resistance.
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)
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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| Publication Number | Publication Date |
|---|---|
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|---|---|---|---|
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|---|---|
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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 |
| 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 |
| CN116550971A (en) * | 2023-03-16 | 2023-08-08 | 西安工业大学 | A kind of Ti3SiC2 modified silicide coating and its preparation method |
-
2009
- 2009-03-04 CN CN200910010565A patent/CN101823900A/en active Pending
Cited By (4)
| 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 |
| CN116550971A (en) * | 2023-03-16 | 2023-08-08 | 西安工业大学 | A kind of Ti3SiC2 modified silicide coating and its preparation method |
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Application publication date: 20100908 |