CN1112167A - Process for preparing high-temp Oxidation resistant ceramic coating by sol and gel method - Google Patents
Process for preparing high-temp Oxidation resistant ceramic coating by sol and gel method Download PDFInfo
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- CN1112167A CN1112167A CN94105090A CN94105090A CN1112167A CN 1112167 A CN1112167 A CN 1112167A CN 94105090 A CN94105090 A CN 94105090A CN 94105090 A CN94105090 A CN 94105090A CN 1112167 A CN1112167 A CN 1112167A
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Abstract
The technology for preparing refractory and antioxidizing ZrO2-Y2O3 ceramic coating on high-temp. alloy substrate includes preparing non-aggregative compound ZrO2-Y2O3 sol, repeated dip-coating for sol-gel transformation on alloy substrate, calcining and compacting to obtain a uniform coating layer of 6 micrometers in thickness. Its antioxidizing temp. is up to 1000 deg.C. The technology is suitable for turbine blade, stainless steel part and others resisting high-temp. oxidation.
Description
The invention belongs to preparation high-temperature oxidation resistant coating technology on alloy substrate.Adopt Sol-Gel method and special roasting system, can obtain the ceramic coating about the thick 6um of reaching, thereby reach the purpose of resistance to high temperature oxidation.
The method of cladding anti oxidation layer has multiple on alloy: as flame plating, plasma spraying or the like, though these methods are widely used, but it is bad that their ubiquities compactness, workpiece shape need height (being not suitable for the spraying of surfaces of complex shape and small-bore internal surface), energy consumption is big, equipment complexity, the problem that cost is high.The Sol-Gel method antithesis, it can reduce sintering temperature, refinement microstructure obtains very purely, stoichiometry is accurate, density is near the ceramic oxide coating of theoretical density.And technology is easy, and equipment is simple, and energy consumption is low, to the surfaces externally and internally shape of workpiece almost without any restriction.The Sol-Gel method has been widely used in nuclear fuel power, ultrafine particle, ceramic fiber, the preparation of various functional films or the like at present.Adopt organic alkoxide, the resistance to high temperature oxidation ceramic coating that can be used for superalloy with the preparation of Sol-Gel method yet there are no any report at home and abroad.
The object of the present invention is to provide a kind of simple and easy to do preparation ZrO
2-Y
2O
3The processing method of high-temperature oxidation resistant ceramic coating is characterized in from organic alkoxide, adopts Sol-Gel technology, with the roasting system of Dip-coating method and the present invention's proposition.Prepared ceramic coating can be used for the protective coating of superalloy turbine blade, also can be used for the resistance to high temperature oxidation coating of stainless steel and other alloy.ZrO
2-Y
2O
3Sol also can prepare from inorganic salt, but because remaining acid ion is difficult to thoroughly remove, the oxidation resistant effect of coating is not very good.And the ZrO that adopts the present invention to prepare from organic alkoxide
2-Y
2O
3Sol does not then contain any acid group and impurity, thereby is more suitable in preparation high performance antioxidation ZrO
2-Y
2O
3Ceramic coating.
The present invention adopts the yttrium isopropoxide preparation to be the aqueous dispersion system (colloidal sol Sol) of colloidal solid in organic solution, and its particle size is 20A-1 μ m.Transfer workpiece Dip-coating after drying dehydration in colloidal sol (Sol) to gel (Gel), pass through roasting again, densification and become ceramic coating.The characteristics of this technology are that coating is very pure, and stoichiometry is accurate, and maturing temperature is low, can obtain the oxide ceramic coating of density near theoretical density about 850 ℃.
Typical process of the present invention is:
Composite S ol is made up of zirconium iso-propoxide and yttrium isopropoxide;
Proportioning: ZrO
270-98%
Y
2O
32-30%
Concentration: 0.1-1M
The Dip time: 10-40 second
Pulling speed:＜1mm/s
Behind the Dip-coating in air the time of gelation: 2-48 hour roasting system:
Heat-up rate:＜160 ℃＜1 ℃/minute
160-280 ℃＜2 ℃/minute
280-480 ℃＜3 ℃/minute
480-850 ℃＜4 ℃/minute
Soaking time: 850 ℃, 15-60 minute
Cooling system: furnace cooling
Atmosphere: laboratory atmospheric environment
Densification: temperature: 900-1100 ℃
Time: 15 minutes-120 minutes
Generally can be after Dip-coating be many times roasting once, the number of times of Dip and roasting number of times are decided on the coat-thickness of requirement, are generally 4-10 time.
Can prepare the ZrO that thickness reaches 6 μ m by above-mentioned technology
2-Y
2O
3Coating is to GH220/CoNiCrAlSiHf/ZrO
2-Y
2O
3It only is 0.2mg/cm that coating increases weight under 1000 ℃ * 100h static oxidation situation
2
Characteristics of the present invention are from organic alkoxide, adopt Sol-Gel technology, with the roasting system of Dip-coating method and the present invention's proposition.Prepared ceramic coating can be used for the protective coating of superalloy turbine blade, the resistance to high temperature oxidation coating that also can be used for stainless steel and other alloy, compare with traditional ceramics coating production (as flame plating and plasma spraying), not only can reduce sintering temperature, refinement microstructure, obtain very pure, stoichiometry is accurate, density is near the ceramic oxide coating of theoretical density, and technology is easy, equipment is simple, and energy consumption is low, to the surfaces externally and internally shape of workpiece almost without any restriction.ZrO
2-Y
2O
3Sol also can prepare from inorganic salt, but because remaining acid ion is difficult to thoroughly remove, and the oxidation resistant effect of coating is not very good, and adopt the ZrO of the present invention from organic alkoxide preparation
2-Y
2O
3Sol does not then contain any acid group and impurity, thereby is more suitable in preparation high performance antioxidation ZrO
2-Y
2O
3Ceramic coating.
The present invention is further illustrated below in conjunction with accompanying drawing.
Figure one is a process flow diagram of the present invention.
Earlier zirconium iso-propoxide and yttrium isopropoxide are dissolved in benzene or aqueous isopropanol (70 ℃) respectively, by the stoicheiometry that calculates two kinds of solution are mixed, workpiece is carried out Dip-coating be placed on air drying in above-mentioned solution, finish Sol-Gel and change, and then by roasting system (see before and the state) roasting of setting.The purpose of roasting is moisture content and the various organic root ball of removing fully among the Gel, and finishes preliminary densification, carries out 1000 ℃ * 30 minutes densification at last and can obtain adhering to the ZrO of good densification
2-Y
2O
3Ceramic coating.The number of times of Dip-coating is decided on the thickness of ceramic coating of final requirement.
SOL by above-mentioned prepared is non-state of aggregation, and colloidal particle is of a size of 20A-1 μ m, and the result is indicated as non-crystalline state through X-ray diffraction studies.
Figure two is the GH220/CoNiCrAlSiHf/ZrO with method preparation of the present invention
2-Y
2O
3Coating is at 1000 ℃, atmospheric environment static oxidation curve.ZrO
2-Y
2O
3Coating is 6 μ m, compares with the CoNiCrAlSiHf coating that does not add ceramic coating, and 100 hours oxidation weight gain reduces by one times, ZrO
2-Y
2O
3The oxidation curve of coating meets logarithmic parabola, and fit equation is: y=0.1173Ln(h)-0.2639.
Embodiment:
Coated ZrO on GH220/CoNiCrAlSiHf
2-Y
2O
3Coating, technology is:
Composite S ol is made up of zirconium iso-propoxide and yttrium isopropoxide;
Proportioning: ZrO
292%
Y
2O
38%
Concentration: 0.2M
The Dip time: 20 seconds
Pulling speed:＜1mm/s
Behind the Dip-coating in air the time of gelation: 24 hours
The roasting system:
Heat-up rate:＜160 ℃＜1 ℃/minute
160-280 ℃＜2 ℃/minute
280-480 ℃＜3 ℃/minute
480-850 ℃＜4 ℃/minute
Soaking time: 850 ℃, 15 minutes
Cooling system: furnace cooling
Atmosphere: laboratory atmospheric environment
Densification: temperature: 1000 ℃
Time: 30 minutes
Dip-coating6 time repeatedly, coat-thickness can reach 6 μ m after densification again.Oxidation-resistance is 1000 ℃ * 100h weightening finish 0.2mg/cm
2And coated ZrO not
2-Y
2O
3GH220/CoNiCrAlSiHf under similarity condition, increase weight to 0.4mg/cm
2More than doubling behind the coated ceramic coating.
Claims (4)
1, a kind of preparation ZrO
2-Y
2O
3The processing method of ceramic coating is characterized in that adopting SOL-GEL technology, from high-purity organic alkoxide preparation Sol (colloidal sol), with Dip-coating (dip-coating) method, drying, roasting and densification can obtain to can be used for the resistance to high temperature oxidation ZrO of superalloy and other alloy material
2-Y
2O
3Ceramic coating.
2, preparation ZrO according to claim 1
2-Y
2O
3The processing method of ceramic coating, it is characterized in that adopting zirconium iso-propoxide and yttrium isopropoxide, dissolving mixes formation Sol(colloidal sol in benzene or Virahol), adopt the Dip-coating method on workpiece, to form one deck sol pellicle, then in the atmospheric environment of laboratory dry 2-48 hour to finish the Sol-Gel(sol-gel) transformation.
3, preparation ZrO according to claim 1 and 2
2-Y
2O
3The processing method of ceramic coating is characterized in that carrying out calcination process by following technology after finishing the Sol-Gel transformation:
Heat-up rate:＜160 ℃＜1 ℃/minute
160-280 ℃＜2 ℃/minute
280-480 ℃＜3 ℃/minute
480-850 ℃＜4 ℃/minute
Soaking time: 850 ℃, 15-60 minute
Cooling system: furnace cooling
Atmosphere: laboratory atmospheric environment
4, preparation ZrO according to claim 1 and 2
2-Y
2O
3The processing method of ceramic coating is characterized in that after carrying out calcination process, carries out the final densification of 1000 ℃/10-120 minute again, the ZrO that can obtain to require
2-Y
2O
3Ceramic coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94105090A CN1056198C (en) | 1994-05-19 | 1994-05-19 | Process for preparing high-temp Oxidation resistant ceramic coating by sol and gel method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94105090A CN1056198C (en) | 1994-05-19 | 1994-05-19 | Process for preparing high-temp Oxidation resistant ceramic coating by sol and gel method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1112167A true CN1112167A (en) | 1995-11-22 |
| CN1056198C CN1056198C (en) | 2000-09-06 |
Family
ID=5031895
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94105090A Expired - Fee Related CN1056198C (en) | 1994-05-19 | 1994-05-19 | Process for preparing high-temp Oxidation resistant ceramic coating by sol and gel method |
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| Country | Link |
|---|---|
| CN (1) | CN1056198C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018056849A1 (en) | 2016-09-20 | 2018-03-29 | Politechnika Krakowska im. Tadeusza Kościuszki | Method of preparing a layer of zirconium(iv) oxide as a catalytic carrier on a metallic substrate |
| CN107880598A (en) * | 2017-11-16 | 2018-04-06 | 华中科技大学 | A kind of platinum rhodium thermocouple surface anti-carbon coating of high adhesion force and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4576874A (en) * | 1984-10-03 | 1986-03-18 | Westinghouse Electric Corp. | Spalling and corrosion resistant ceramic coating for land and marine combustion turbines |
| CN1004159B (en) * | 1985-04-01 | 1989-05-10 | 株式会社日立制作所 | Combustion device of gas turbine |
| GB8809608D0 (en) * | 1988-04-22 | 1988-05-25 | Alcan Int Ltd | Sol-gel method of making ceramics |
-
1994
- 1994-05-19 CN CN94105090A patent/CN1056198C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018056849A1 (en) | 2016-09-20 | 2018-03-29 | Politechnika Krakowska im. Tadeusza Kościuszki | Method of preparing a layer of zirconium(iv) oxide as a catalytic carrier on a metallic substrate |
| CN107880598A (en) * | 2017-11-16 | 2018-04-06 | 华中科技大学 | A kind of platinum rhodium thermocouple surface anti-carbon coating of high adhesion force and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1056198C (en) | 2000-09-06 |
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