CN106567077B - A kind of preparation method of high-temp. alloy surface heat barrier - Google Patents
A kind of preparation method of high-temp. alloy surface heat barrier Download PDFInfo
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
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Abstract
The invention discloses a kind of preparation methods of high-temp. alloy surface heat barrier; the following steps are included: preparing nanometer zirconic acid gadolinium ceramic powder first; then by high temperature alloy matrix after pre-grinding, polishing, cleaning treatment; adhesive layer is deposited on high temperature alloy matrix using the method for Low Pressure Condition Plasma Sprayed, then using plasma spray coating process in the ceramic coated protective layer of tie layer surface；Nanometer Gd is finally deposited on ceramic protective layer using electro beam physics vapour deposition method2Zr2O7Ceramic layer is as thermal barrier coating；Then ceramic heat-barrier coating surface obtained removes surface dust and particle with vacuum cleaner, and is placed in oven and dried.Thermal barrier coating thermal conductivity produced by the present invention is small, can effectively improve the high temperature resistance of alloy, and thermal barrier coating is fine and close, not easy to crack, antioxygenic property and corrosion resistance and good.
Description
Technical field:
The present invention relates to metal surface modification fields, are specifically related to a kind of preparation side of high-temp. alloy surface heat barrier
Method.
Background technique:
Now, the main direction of development of gas-turbine unit is ignition temperature before improving engine turbine, increases and have an high regard for
Than and to promote turbine engine components including the thermal efficiency under harsh Service Environment such as corrosion and oxidation.With engine combustion
The raising of temperature, thrust ratio and the thermal efficiency, fuel gas temperature and gaseous-pressure in engine thermal end pieces, especially combustion chamber are not
It is disconnected to improve.Last from last century forties the to last century, gaseous-pressure ratio improves nearly 3 times, and fuel gas temperature is more than 1650 DEG C.For
Reach improve efficiency, energy saving requirement, the operating temperature of combustion gas turbine almost with the rate of 15 DEG C/a it is quick on
It rises, it is contemplated that be up to 1930 DEG C quickly.Temperature high in this way alreadys exceed the fusing point of existing alloy, and novel high-temperature alloy is heat-resisting
The growth of performance only about 5 DEG C/a, therefore, it is necessary to using corresponding measure.On the one hand, using vacuum melting and hot investment casting
Etc. advanced technology of preparing and continue the high-temperature material of development of new, improve the heat resistance of high temperature alloy, as directional solidification is closed
Gold and single crystal alloy；On the other hand, using advanced cooling technology, such as the design of blade cooling air film and the improvement of manufacturing process.
However due to being limited by its fusing point, the potentiality for further increasing high temperature alloy operating temperature are extremely limited.It causes
Power while further Development of Novel alloy and cooling technology, it is expected to seek other approach by engine designers, to reduce
The service temperature and reduction engine blade of high temperature alloy fail because of caused by overheat, wherein developing high-temp heat barrier coating technology
Be it is yearning, with development prospect.
The heat-protection system that thermal barrier coating is made of the priming coat of ceramic oxide surface layer and cementation.It utilizes pottery
The excellent high temperature resistant of ceramic material, resistance to erosion, anticorrosive and low heat conductivity energy, improve the allowable work temperature of metal parts, enhancing
The high-temperature resistance of hot-end component extends the service life of hot-end component, improves the working efficiency of engine.Therefore how to be made
The thermal barrier coating fine and close, antioxygenic property is good, thermal conductivity is low becomes the key for improving high temperature alloy heat resistance.
Summary of the invention:
The object of the present invention is to provide a kind of preparation methods of high-temp. alloy surface heat barrier, and this method is easy to operate,
Low for equipment requirements, thermal barrier coating thermal conductivity obtained is low, and stability is good, can effectively improve the high temperature resistance and antioxygen of alloy
Change performance.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of high-temp. alloy surface heat barrier, comprising the following steps:
(1) preparation of nanometer zirconic acid gadolinium ceramic powder:
A) laboratory temperature is adjusted with air-conditioning, is that 1:1 weighs Gd (NO respectively according to Gd:Zr molar ratio3)3·6H2O and
ZrOCl2·8H2O adds deionized water to be diluted to the mixed solution containing Gd and Zr, stirs evenly；
B) weak aqua ammonia is taken, will be instilled dropwise in the weak aqua ammonia of stirring, be added dropwise containing Gd and Zr mixed solution with peristaltic pump
Afterwards, stirring, ageing are closed；
C) precipitating after ageing is subjected to centrifuge washing, be first washed with deionized to after silver nitrate is added to centrifugation
In supernatant liquor without white precipitate until, then again use washes of absolute alcohol 2-3 times；Finally by the anhydrous second of the precipitating after washing
It is put into reaction kettle after alcohol dilution and reacts 20-24h at 180-200 DEG C；
D) precipitating is washed 1-2 times after reaction with dehydrated alcohol, is put into drying box, it is dry at 50-70 DEG C, it is dry
Grinding after complete, and be sieved in 200 mesh screens, then in Muffle kiln roasting, obtain Gd2Zr2O7Nano-powder；
E) Gd made from step d) is taken2Zr2O7Nano-powder is placed in graphite jig, and sleeve lining and upper push-down head respectively pad
One layer of carbon paper, by nano-powder it is die-filling after with graphite jig together in drying box it is dry, then on desk type powder dry press
Precompressed, preload pressure 1-2MPa；
F) Gd will be housed2Zr2O7After the graphite jig of nano-powder is correctly placed in discharge plasma sintering furnace, close
Closed furnace door starts to vacuumize, when vacuum degree be less than 6Pa when, start to pressurize, pressure 60-80MPa, set program power and
Time starts to be sintered, and sintering finishes, and is down to 30 DEG C hereinafter, beginning release, is unsnatched to whole pressure to in-furnace temperature, deflation is opened
Fire door demoulds, and samples, and smashing and grinding obtains a nanometer Gd2Zr2O7Ceramic powder；
(2) by high temperature alloy matrix after pre-grinding, polishing, cleaning treatment, using the method for Low Pressure Condition Plasma Sprayed
Adhesive layer is deposited on high temperature alloy matrix, then using plasma spray coating process in the ceramic coated protective layer of tie layer surface；
(3) then the high temperature alloy matrix surface of adhesive layer and ceramic protective layer will be coated under nitrogen or argon
It is cleaned using pulse laser；And the material surface after cleaning is subjected to laser roughening processing under vacuum or argon gas protection, finally
Nanometer Gd is deposited on ceramic protective layer using electro beam physics vapour deposition method2Zr2O7Ceramic layer is as thermal barrier coating；
(4) surface dust and particle are removed to the vacuum cleaner of ceramic heat-barrier coating surface made from step (3), and put
Enter dry in baking oven.
As a preferred embodiment of the above technical solution, in step a), laboratory temperature is 5-20 DEG C.
As a preferred embodiment of the above technical solution, in step b), the concentration of the mixed solution containing Gd and Zr is 0.03-
0.05mol/L, the concentration of weak aqua ammonia are 0.4-0.6mol/L, and the volume ratio of weak aqua ammonia and the mixed solution containing Gd and Zr is 2:1.
As a preferred embodiment of the above technical solution, in step b), the time of the ageing is 20-24h.
As a preferred embodiment of the above technical solution, in step d), the temperature of the roasting is 800-1000 DEG C, the time of roasting
For 2-5h.
As a preferred embodiment of the above technical solution, in step e), the temperature of the drying is 180-200 DEG C, the dry time
For 4-6h.
As a preferred embodiment of the above technical solution, it in step f), when sintering, is warming up to first with the rate of 30-40 DEG C/min
600 DEG C, it then is warming up to 1300-1350 DEG C with the rate of 40-60 DEG C/min, 3-5min is kept the temperature, is then dropped by 30-50 DEG C/min
To 600 DEG C, sintering finishes temperature.
As a preferred embodiment of the above technical solution, in step (2), the adhesive layer is NiCrAlY, with a thickness of 0.05-
0.08mm。
As a preferred embodiment of the above technical solution, in step (2), the protective layer is aluminium oxide, titanium oxide, silica, oxygen
Change the compound of one of zirconium or a variety of compositions, protective layer with a thickness of 0.001-0.002mm.
As a preferred embodiment of the above technical solution, in step (3), the thermal barrier coating with a thickness of 0.07-0.12mm.
Compared with prior art, the invention has the following advantages:
The present invention successively sprays adhesive layer, ceramic protective layer and thermal barrier coating in high-temperature alloy surface, ties between layers
It is good with joint efforts, not easily to fall off, the heat resistance and stability of the high temperature alloy that can effectively improve；
The present invention is modified nano-powder, nanometer Gd obtained2Zr2O7Ceramic powder size is small, better crystallinity degree, point
Scattered property is good, and thermal barrier coating compactness obtained is good, and not easy to crack, thermal conductivity is low, can effectively improve the high temperature resistance of alloy, and
The preparation method time is short, high-efficient, energy saving.
Specific embodiment:
In order to better understand the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of preparation method of high-temp. alloy surface heat barrier, comprising the following steps:
(1) preparation of nanometer zirconic acid gadolinium ceramic powder:
A) laboratory temperature is adjusted with air-conditioning, is that 1:1 weighs Gd (NO respectively according to Gd:Zr molar ratio3)3·6H2O and
ZrOCl2·8H2O adds deionized water to be diluted to the mixed solution containing Gd and Zr, stirs evenly, and obtaining concentration is containing for 0.03mol/L
Gd and Zr mixed solution；
B) taking concentration is the weak aqua ammonia of 0.4mol/L, will instill dropwise the dilute of stirring containing Gd and Zr mixed solution with peristaltic pump
In ammonium hydroxide, after being added dropwise, stirring is closed, is aged 20h, wherein weak aqua ammonia is with the volume ratio containing Gd and the mixed solution of Zr
2:1；
C) precipitating after ageing is subjected to centrifuge washing, be first washed with deionized to after silver nitrate is added to centrifugation
In supernatant liquor without white precipitate until, then again use washes of absolute alcohol 2-3 times；Finally by the anhydrous second of the precipitating after washing
It is put into reaction kettle after alcohol dilution and reacts 20h at 180 DEG C；
D) precipitating is washed 1-2 times after reaction with dehydrated alcohol, is put into drying box, it is dry at 50 DEG C, it has dried
After grind, and be sieved in 200 mesh screens, then in Muffle furnace, roast 2h at 800 DEG C, obtain Gd2Zr2O7Nano powder
Body；
E) Gd made from step d) is taken2Zr2O7Nano-powder is placed in graphite jig, and sleeve lining and upper push-down head respectively pad
One layer of carbon paper, by nano-powder it is die-filling after with the graphite jig together dry 4h at 180 DEG C in drying box, then in desk type powder
Precompressed on dry press, preload pressure 1-2MPa；
F) Gd will be housed2Zr2O7After the graphite jig of nano-powder is correctly placed in discharge plasma sintering furnace, close
Closed furnace door starts to vacuumize, when vacuum degree be less than 6Pa when, start to pressurize, pressure 60MPa, set program power and when
Between, start to be sintered, when sintering, is warming up to 600 DEG C first with the rate of 30 DEG C/min, is then warming up to the rate of 40 DEG C/min
1300 DEG C, 3min is kept the temperature, then cools to 600 DEG C by 30 DEG C/min, sintering finishes, and is down to 30 DEG C hereinafter, opening to in-furnace temperature
Beginning release is unsnatched to whole pressure, is deflated, and blow-on door demoulds, and is sampled, and smashing and grinding obtains a nanometer Gd2Zr2O7Ceramic powder；
(2) by high temperature alloy matrix after pre-grinding, polishing, cleaning treatment, using the method for Low Pressure Condition Plasma Sprayed
The NiCrAlY adhesive layer with a thickness of 0.05mm is deposited as on high temperature alloy matrix, then using plasma spray coating process viscous
Tie the ceramic protective layer that layer surface coating thickness is 0.001mm；
(3) then the high temperature alloy matrix surface of adhesive layer and ceramic protective layer will be coated under nitrogen or argon
It is cleaned using pulse laser；And the material surface after cleaning is subjected to laser roughening processing under vacuum or argon gas protection, finally
The nanometer Gd that deposition thickness is 0.07mm on ceramic protective layer using electro beam physics vapour deposition method2Zr2O7Ceramic layer is made
For thermal barrier coating；
(4) surface dust and particle are removed to the vacuum cleaner of ceramic heat-barrier coating surface made from step (3), and put
Enter dry in baking oven.
Embodiment 2
A kind of preparation method of high-temp. alloy surface heat barrier, comprising the following steps:
(1) preparation of nanometer zirconic acid gadolinium ceramic powder:
A) laboratory temperature is adjusted with air-conditioning, is that 1:1 weighs Gd (NO respectively according to Gd:Zr molar ratio3)3·6H2O and
ZrOCl2·8H2O adds deionized water to be diluted to the mixed solution containing Gd and Zr, stirs evenly, and obtaining concentration is containing for 0.05mol/L
Gd and Zr mixed solution；
B) taking concentration is the weak aqua ammonia of 0.6mol/L, will instill dropwise the dilute of stirring containing Gd and Zr mixed solution with peristaltic pump
In ammonium hydroxide, after being added dropwise, stirring is closed, ageing is for 24 hours, wherein weak aqua ammonia is with the volume ratio containing Gd and the mixed solution of Zr
2:1；
C) precipitating after ageing is subjected to centrifuge washing, be first washed with deionized to after silver nitrate is added to centrifugation
In supernatant liquor without white precipitate until, then again use washes of absolute alcohol 2-3 times；Finally by the anhydrous second of the precipitating after washing
It is put into reaction kettle after alcohol dilution and is reacted for 24 hours at 200 DEG C；
D) precipitating is washed 1-2 times after reaction with dehydrated alcohol, is put into drying box, it is dry at 70 DEG C, it has dried
After grind, and be sieved in 200 mesh screens, then in Muffle furnace, roast 5h at 1000 DEG C, obtain Gd2Zr2O7Nano powder
Body；
E) Gd made from step d) is taken2Zr2O7Nano-powder is placed in graphite jig, and sleeve lining and upper push-down head respectively pad
One layer of carbon paper, by nano-powder it is die-filling after with the graphite jig together dry 6h at 200 DEG C in drying box, then in desk type powder
Precompressed on dry press, preload pressure 1-2MPa；
F) Gd will be housed2Zr2O7After the graphite jig of nano-powder is correctly placed in discharge plasma sintering furnace, close
Closed furnace door starts to vacuumize, when vacuum degree be less than 6Pa when, start to pressurize, pressure 80MPa, set program power and when
Between, start to be sintered, when sintering, is warming up to 600 DEG C first with the rate of 40 DEG C/min, is then warming up to the rate of 60 DEG C/min
1350 DEG C, 5min is kept the temperature, then cools to 600 DEG C by 50 DEG C/min, sintering finishes, and is down to 30 DEG C hereinafter, opening to in-furnace temperature
Beginning release is unsnatched to whole pressure, is deflated, and blow-on door demoulds, and is sampled, and smashing and grinding obtains a nanometer Gd2Zr2O7Ceramic powder；
(2) by high temperature alloy matrix after pre-grinding, polishing, cleaning treatment, using the method for Low Pressure Condition Plasma Sprayed
The NiCrAlY adhesive layer with a thickness of 0.08mm is deposited as on high temperature alloy matrix, then using plasma spray coating process viscous
Tie the ceramic protective layer that layer surface coating thickness is 0.002mm；
(3) then the high temperature alloy matrix surface of adhesive layer and ceramic protective layer will be coated under nitrogen or argon
It is cleaned using pulse laser；And the material surface after cleaning is subjected to laser roughening processing under vacuum or argon gas protection, finally
The nanometer Gd that deposition thickness is 0.12mm on ceramic protective layer using electro beam physics vapour deposition method2Zr2O7Ceramic layer is made
For thermal barrier coating；
(4) surface dust and particle are removed to the vacuum cleaner of ceramic heat-barrier coating surface made from step (3), and put
Enter dry in baking oven.
Embodiment 3
A kind of preparation method of high-temp. alloy surface heat barrier, comprising the following steps:
(1) preparation of nanometer zirconic acid gadolinium ceramic powder:
A) laboratory temperature is adjusted with air-conditioning, is that 1:1 weighs Gd (NO respectively according to Gd:Zr molar ratio3)3·6H2O and
ZrOCl2·8H2O adds deionized water to be diluted to the mixed solution containing Gd and Zr, stirs evenly, and obtaining concentration is 0.035mol/L's
Containing Gd and Zr mixed solution；
B) taking concentration is the weak aqua ammonia of 0.45mol/L, and stirring will be instilled dropwise containing Gd and Zr mixed solution with peristaltic pump
In weak aqua ammonia, after being added dropwise, stirring is closed, is aged 21h, wherein the volume ratio of weak aqua ammonia and the mixed solution containing Gd and Zr
For 2:1；
C) precipitating after ageing is subjected to centrifuge washing, be first washed with deionized to after silver nitrate is added to centrifugation
In supernatant liquor without white precipitate until, then again use washes of absolute alcohol 2-3 times；Finally by the anhydrous second of the precipitating after washing
It is put into reaction kettle after alcohol dilution and reacts 21h at 185 DEG C；
D) precipitating is washed 1-2 times after reaction with dehydrated alcohol, is put into drying box, it is dry at 55 DEG C, it has dried
After grind, and be sieved in 200 mesh screens, then in Muffle furnace, roast 3h at 850 DEG C, obtain Gd2Zr2O7Nano powder
Body；
E) Gd made from step d) is taken2Zr2O7Nano-powder is placed in graphite jig, and sleeve lining and upper push-down head respectively pad
One layer of carbon paper, by nano-powder it is die-filling after with the graphite jig together dry 4.5h at 185 DEG C in drying box, then in desk-top powder
Precompressed on last dry press, preload pressure 1-2MPa；
F) Gd will be housed2Zr2O7After the graphite jig of nano-powder is correctly placed in discharge plasma sintering furnace, close
Closed furnace door starts to vacuumize, when vacuum degree be less than 6Pa when, start to pressurize, pressure 65MPa, set program power and when
Between, start to be sintered, when sintering, is warming up to 600 DEG C first with the rate of 33 DEG C/min, is then warming up to the rate of 45 DEG C/min
1310 DEG C, 3min is kept the temperature, then cools to 600 DEG C by 35 DEG C/min, sintering finishes, and is down to 30 DEG C hereinafter, opening to in-furnace temperature
Beginning release is unsnatched to whole pressure, is deflated, and blow-on door demoulds, and is sampled, and smashing and grinding obtains a nanometer Gd2Zr2O7Ceramic powder；
(2) by high temperature alloy matrix after pre-grinding, polishing, cleaning treatment, using the method for Low Pressure Condition Plasma Sprayed
The NiCrAlY adhesive layer with a thickness of 0.06mm is deposited as on high temperature alloy matrix, then using plasma spray coating process viscous
Tie the ceramic protective layer that layer surface coating thickness is 0.001mm；
(3) then the high temperature alloy matrix surface of adhesive layer and ceramic protective layer will be coated under nitrogen or argon
It is cleaned using pulse laser；And the material surface after cleaning is subjected to laser roughening processing under vacuum or argon gas protection, finally
The nanometer Gd that deposition thickness is 0.08mm on ceramic protective layer using electro beam physics vapour deposition method2Zr2O7Ceramic layer is made
For thermal barrier coating；
(4) surface dust and particle are removed to the vacuum cleaner of ceramic heat-barrier coating surface made from step (3), and put
Enter dry in baking oven.
Embodiment 4
A kind of preparation method of high-temp. alloy surface heat barrier, comprising the following steps:
(1) preparation of nanometer zirconic acid gadolinium ceramic powder:
A) laboratory temperature is adjusted with air-conditioning, is that 1:1 weighs Gd (NO respectively according to Gd:Zr molar ratio3)3·6H2O and
ZrOCl2·8H2O adds deionized water to be diluted to the mixed solution containing Gd and Zr, stirs evenly, and obtaining concentration is containing for 0.04mol/L
Gd and Zr mixed solution；
B) taking concentration is the weak aqua ammonia of 0.5mol/L, will instill dropwise the dilute of stirring containing Gd and Zr mixed solution with peristaltic pump
In ammonium hydroxide, after being added dropwise, stirring is closed, is aged 22h, wherein weak aqua ammonia is with the volume ratio containing Gd and the mixed solution of Zr
2:1；
C) precipitating after ageing is subjected to centrifuge washing, be first washed with deionized to after silver nitrate is added to centrifugation
In supernatant liquor without white precipitate until, then again use washes of absolute alcohol 2-3 times；Finally by the anhydrous second of the precipitating after washing
It is put into reaction kettle after alcohol dilution and reacts 22h at 190 DEG C；
D) precipitating is washed 1-2 times after reaction with dehydrated alcohol, is put into drying box, it is dry at 60 DEG C, it has dried
After grind, and be sieved in 200 mesh screens, then in Muffle furnace, roast 4h at 900 DEG C, obtain Gd2Zr2O7Nano powder
Body；
E) Gd made from step d) is taken2Zr2O7Nano-powder is placed in graphite jig, and sleeve lining and upper push-down head respectively pad
One layer of carbon paper, by nano-powder it is die-filling after with the graphite jig together dry 5h at 190 DEG C in drying box, then in desk type powder
Precompressed on dry press, preload pressure 1-2MPa；
F) Gd will be housed2Zr2O7After the graphite jig of nano-powder is correctly placed in discharge plasma sintering furnace, close
Closed furnace door starts to vacuumize, when vacuum degree be less than 6Pa when, start to pressurize, pressure 70MPa, set program power and when
Between, start to be sintered, when sintering, is warming up to 600 DEG C first with the rate of 36 DEG C/min, is then warming up to the rate of 50 DEG C/min
1320 DEG C, 4min is kept the temperature, then cools to 600 DEG C by 40 DEG C/min, sintering finishes, and is down to 30 DEG C hereinafter, opening to in-furnace temperature
Beginning release is unsnatched to whole pressure, is deflated, and blow-on door demoulds, and is sampled, and smashing and grinding obtains a nanometer Gd2Zr2O7Ceramic powder；
(2) by high temperature alloy matrix after pre-grinding, polishing, cleaning treatment, using the method for Low Pressure Condition Plasma Sprayed
The NiCrAlY adhesive layer with a thickness of 0.07mm is deposited as on high temperature alloy matrix, then using plasma spray coating process viscous
Tie the ceramic protective layer that layer surface coating thickness is 0.001mm；
(3) then the high temperature alloy matrix surface of adhesive layer and ceramic protective layer will be coated under nitrogen or argon
It is cleaned using pulse laser；And the material surface after cleaning is subjected to laser roughening processing under vacuum or argon gas protection, finally
The nanometer Gd that deposition thickness is 0.09mm on ceramic protective layer using electro beam physics vapour deposition method2Zr2O7Ceramic layer is made
For thermal barrier coating；
(4) surface dust and particle are removed to the vacuum cleaner of ceramic heat-barrier coating surface made from step (3), and put
Enter dry in baking oven.
Embodiment 5
A kind of preparation method of high-temp. alloy surface heat barrier, comprising the following steps:
(1) preparation of nanometer zirconic acid gadolinium ceramic powder:
A) laboratory temperature is adjusted with air-conditioning, is that 1:1 weighs Gd (NO respectively according to Gd:Zr molar ratio3)3·6H2O and
ZrOCl2·8H2O adds deionized water to be diluted to the mixed solution containing Gd and Zr, stirs evenly, and obtaining concentration is 0.045mol/L's
Containing Gd and Zr mixed solution；
B) taking concentration is the weak aqua ammonia of 0.55mol/L, and stirring will be instilled dropwise containing Gd and Zr mixed solution with peristaltic pump
In weak aqua ammonia, after being added dropwise, stirring is closed, is aged 23h, wherein the volume ratio of weak aqua ammonia and the mixed solution containing Gd and Zr
For 2:1；
C) precipitating after ageing is subjected to centrifuge washing, be first washed with deionized to after silver nitrate is added to centrifugation
In supernatant liquor without white precipitate until, then again use washes of absolute alcohol 2-3 times；Finally by the anhydrous second of the precipitating after washing
It is put into reaction kettle after alcohol dilution and reacts 23h at 195 DEG C；
D) precipitating is washed 1-2 times after reaction with dehydrated alcohol, is put into drying box, it is dry at 65 DEG C, it has dried
After grind, and be sieved in 200 mesh screens, then in Muffle furnace, roast 4h at 950 DEG C, obtain Gd2Zr2O7Nano powder
Body；
E) Gd made from step d) is taken2Zr2O7Nano-powder is placed in graphite jig, and sleeve lining and upper push-down head respectively pad
One layer of carbon paper, by nano-powder it is die-filling after with the graphite jig together dry 5.5h at 195 DEG C in drying box, then in desk-top powder
Precompressed on last dry press, preload pressure 1-2MPa；
F) Gd will be housed2Zr2O7After the graphite jig of nano-powder is correctly placed in discharge plasma sintering furnace, close
Closed furnace door starts to vacuumize, when vacuum degree be less than 6Pa when, start to pressurize, pressure 75MPa, set program power and when
Between, start to be sintered, when sintering, is warming up to 600 DEG C first with the rate of 38 DEG C/min, is then warming up to the rate of 55 DEG C/min
1340 DEG C, 4min is kept the temperature, then cools to 600 DEG C by 45 DEG C/min, sintering finishes, and is down to 30 DEG C hereinafter, opening to in-furnace temperature
Beginning release is unsnatched to whole pressure, is deflated, and blow-on door demoulds, and is sampled, and smashing and grinding obtains a nanometer Gd2Zr2O7Ceramic powder；
(2) by high temperature alloy matrix after pre-grinding, polishing, cleaning treatment, using the method for Low Pressure Condition Plasma Sprayed
The NiCrAlY adhesive layer with a thickness of 0.07mm is deposited as on high temperature alloy matrix, then using plasma spray coating process viscous
Tie the ceramic protective layer that layer surface coating thickness is 0.002mm；
(3) then the high temperature alloy matrix surface of adhesive layer and ceramic protective layer will be coated under nitrogen or argon
It is cleaned using pulse laser；And the material surface after cleaning is subjected to laser roughening processing under vacuum or argon gas protection, finally
The nanometer Gd that deposition thickness is 0.10mm on ceramic protective layer using electro beam physics vapour deposition method2Zr2O7Ceramic layer is made
For thermal barrier coating；
(4) surface dust and particle are removed to the vacuum cleaner of ceramic heat-barrier coating surface made from step (3), and put
Enter dry in baking oven.
Claims (8)
1. a kind of preparation method of high-temp. alloy surface heat barrier, which comprises the following steps:
(1) preparation of nanometer zirconic acid gadolinium ceramic powder:
A) laboratory temperature is adjusted with air-conditioning, is that 1:1 weighs Gd (NO respectively according to Gd:Zr molar ratio3)3·6H2O and
ZrOCl2·8H2O adds deionized water to be diluted to the mixed solution containing Gd and Zr, stirs evenly；
B) weak aqua ammonia is taken, will be instilled dropwise containing Gd and Zr mixed solution in the weak aqua ammonia of stirring with peristaltic pump, after being added dropwise, is closed
Stirring is closed, is aged；Wherein, the concentration of the mixed solution containing Gd and Zr is 0.03-0.05mol/L, and the concentration of weak aqua ammonia is
The volume ratio of 0.4-0.6mol/L, weak aqua ammonia and the mixed solution containing Gd and Zr is 2:1；
C) by after ageing precipitating carry out centrifuge washing, be first washed with deionized to by silver nitrate be added to centrifugation after upper layer
In clear liquid without white precipitate until, then again use washes of absolute alcohol 2-3 times；It is finally that the precipitating dehydrated alcohol after washing is dilute
It is put into after releasing in reaction kettle and reacts 20-24h at 180-200 DEG C；
D) precipitating is washed 1-2 times after reaction with dehydrated alcohol, is put into drying box, it is dry at 50-70 DEG C, after having dried
Grinding, and be sieved in 200 mesh screens, then in Muffle kiln roasting, obtain Gd2Zr2O7Nano-powder；
E) Gd made from step d) is taken2Zr2O7Nano-powder is placed in graphite jig, and sleeve lining and upper push-down head respectively pad one layer
Carbon paper, by nano-powder it is die-filling after with graphite jig dry, the then precompressed on desk type powder dry press in drying box together,
Preload pressure is 1-2MPa；
F) Gd will be housed2Zr2O7After the graphite jig of nano-powder is correctly placed in discharge plasma sintering furnace, furnace is closed
Door start to vacuumize, when vacuum degree be less than 6Pa when, start to pressurize, pressure 60-80MPa, set program power and when
Between, start to be sintered, sintering finishes, to in-furnace temperature be down to 30 DEG C hereinafter, start release, unsnatched to whole pressure, deflate, blow-on
Door demoulds, and samples, and smashing and grinding obtains a nanometer Gd2Zr2O7Ceramic powder；Wherein, when sintering, first with 30-40 DEG C/min's
Rate is warming up to 600 DEG C, is then warming up to 1300-1350 DEG C with the rate of 40-60 DEG C/min, keeps the temperature 3-5min, then presses 30-
50 DEG C/min cools to 600 DEG C, and sintering finishes；
(2) by high temperature alloy matrix after pre-grinding, polishing, cleaning treatment, using the method for Low Pressure Condition Plasma Sprayed in height
Adhesive layer is deposited on temperature alloy matrix, then using plasma spray coating process in the ceramic coated protective layer of tie layer surface；
(3) then the high temperature alloy matrix surface for being coated with adhesive layer and ceramic protective layer is used under nitrogen or argon
Pulse laser cleaning；And the material surface after cleaning is subjected to laser roughening processing under vacuum or argon gas protection, finally utilize
Electro beam physics vapour deposition method deposits nanometer Gd on ceramic protective layer2Zr2O7Ceramic layer is as thermal barrier coating；
(4) surface dust and particle are removed to the vacuum cleaner of ceramic heat-barrier coating surface made from step (3), and is put into baking
It is dry in case.
2. a kind of preparation method of high-temp. alloy surface heat barrier as described in claim 1, it is characterised in that: step a)
In, laboratory temperature is 5-20 DEG C.
3. a kind of preparation method of high-temp. alloy surface heat barrier as described in claim 1, it is characterised in that: step b)
In, the time of the ageing is 20-24h.
4. a kind of preparation method of high-temp. alloy surface heat barrier as described in claim 1, it is characterised in that: step d)
In, the temperature of the roasting is 800-1000 DEG C, and the time of roasting is 2-5h.
5. a kind of preparation method of high-temp. alloy surface heat barrier as described in claim 1, it is characterised in that: step e)
In, the temperature of the drying is 180-200 DEG C, and the dry time is 4-6h.
6. a kind of preparation method of high-temp. alloy surface heat barrier as described in claim 1, it is characterised in that: step (2)
In, the adhesive layer is NiCrAlY, with a thickness of 0.05-0.08mm.
7. a kind of preparation method of high-temp. alloy surface heat barrier as described in claim 1, it is characterised in that: step (2)
In, the protective layer is the compound of one of aluminium oxide, titanium oxide, silica, zirconium oxide or a variety of compositions, protective layer
With a thickness of 0.001-0.002mm.
8. a kind of preparation method of high-temp. alloy surface heat barrier as described in claim 1, it is characterised in that: step (3)
In, the thermal barrier coating with a thickness of 0.07-0.12mm.
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