CN110256092A - A kind of heat barrier coat material and preparation method thereof - Google Patents
A kind of heat barrier coat material and preparation method thereof Download PDFInfo
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- CN110256092A CN110256092A CN201910696758.6A CN201910696758A CN110256092A CN 110256092 A CN110256092 A CN 110256092A CN 201910696758 A CN201910696758 A CN 201910696758A CN 110256092 A CN110256092 A CN 110256092A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62222—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic coatings
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
Abstract
The invention belongs to aero-engine key coat preparing technology field, specially a kind of preparation method of aero-turbine thermal barrier coating.The reaction raw materials powder and RE oxide powder of thermal barrier coating are uniformly mixed, it is preset on alloy or metallic matrix, control laser facula size, power, the parameters such as time carry out laser irradiation or sintering, laser resonant intensifies rare earth sensitized ions, realize energy transfer, lasting laser energy supply, intensify the ion intensified generation again and multistep cascade reaction and energy transfer, to induce mixed raw material that high temperature solid state reaction occurs, self- propagating grows one layer of thermal barrier coating on matrix, the input of the method for the present invention laser energy is low, rapid reaction, the thermal barrier coating and substrate adhesion of preparation are high, coating uniform crackle is few, with preferable thermal shock resistance, and the preparation method raw material availability is high, energy conservation and environmental protection, it is suitble to large area industrialized production.
Description
Technical field
The invention belongs to laser processing technologys and field of energy source materials, and in particular to a kind of heat barrier coat material and its preparation
Method.
Background technique
Thermal barrier coating (Thermal Barrier Coatings, TBCs) is by high temperature resistant, low thermally conductive, erosion-resisting pottery
Ceramic material is coated in workpiece surface, a kind of thermal protection to reduce workpiece surface temperature under high-temperature service environment in a manner of coating
Technology is mainly used in gas engine turbo blade at present, can significantly improve the working efficiency and thrust of engine, simultaneously
The operating temperature of blade alloy can be reduced, is advanced aero engine to increase substantially the life and reliability of engine
Indispensable a key technology.With the rapid development of aerospace industry, fuel gas inlet temperature before engine turbine blade
Degree has reached 1700 DEG C, higher and higher to refractory layer and paint-on technique requirement, is widely used in thermal barrier coating system at present
Be 6-8wt.%Y2O3-ZrO2(6-8wt.%YSZ) material, there are phase transformation failure, sintering is serious, thermal expansion mismatches and
A series of serious problems such as thermal conductivity height.A2B2O7Type rare earth zirconate material has thermal conductivity more lower than 6-8wt.%, more preferably
Heat insulation, while at high temperature have good chemical stability and phase stability, be the best of heat-barrier coating ceramic layer
One of candidate material.
Thermal barrier coating technology of preparing is the key that improve thermal barrier coating performance, and YSZ thermal barrier coating mostly uses electron beam at present
Physical vapour deposition (PVD) (EB-PVD) and plasma spraying (APS), but with the harshness of application environment, coat preparing technology needs not
It is disconnected to improve.A2B2O7The preparation of type thermal barrier coating mainly uses the method for fractional steps to carry out: 1. are closed using solid phase method, sol method or hydro-thermal method
At A2B2O7Type ceramic material；2. by the A of synthesis2B2O7Type ceramic material is processed into the small A of epigranular, partial size2B2O7Powder；
3. using coating processes by A2B2O7Powder coating obtains A on basis material2B2O7Type heat barrier coat material.This preparation side
Method is in addition to complex steps, in synthesis A2B2O7Also following problems: 1. Solid phase synthesis A can be faced when type ceramic material2B2O7Type pottery
Reaction temperature is high when ceramic material, and the pyroreaction time is long, requires equipment energy consumption very big；2. sol method technique is cumbersome, raw material is wanted
It asks high and organic pollution can be generated；Hydro-thermal method equipment requirement is high, and technical difficulty is big, and security performance is low etc..Therefore, novel thermal boundary
The preparation of coating material is greatly limited, and is badly in need of a kind of simple process, the growth that high-efficient, pollution is small, the period is short
A2B2O7The preparation method of type thermal barrier coating.
Summary of the invention
It is an object of the invention to propose a kind of novel solid oxide fuel cell solid electrolyte and a kind of simple
Efficient solid electrolyte preparation method, to solve the above problem in the presence of the prior art.
The present invention is achieved by the following technical solutions:
A kind of heat barrier coat material, general molecular formula A2B2O7, wherein A Sc, Y, La, Nd, Eu, Gd, Dy, Er, Yb
At least one of with Lu, at least one of B Ti, Zr, Ce and Hf.
Preferably, the molecular formula of the heat barrier coat material is Yb2Zr2O7。
A kind of preparation method of heat barrier coat material as the aforementioned comprising following steps:
S1, by oxide AOmWith oxide BOnAfter being mixed by underhand polish or ball milling, with dehydrated alcohol, acetone or go
Ionized water is that medium carries out wet ball grinding, until partial size is no more than 1 μm, after product is taken out, drying, is ground at 60~80 DEG C
Material, the abrasive material is ground, and obtains reaction powder；
S2, it after being compacted the reaction powder, is sintered under laser irradiation, obtains the ceramic electrolyte material
Material；
Wherein, m and n is integer.
Preferably, further include the steps that being granulated reaction powder in step S1, specifically:
The adhesive solution for being 1~10% by binder making mass fraction divides 2~3 times and is added to the reaction powder
It in end, ground, cross 20~50 meshes；
Include the steps that row is viscous in step S2, specifically:
Product after sieving is compacted, and it is viscous to carry out row by the method for heating or laser irradiation.
Preferably, the binder includes at least one of PVA, methoxy silane, polyurethane, silicone.
Preferably, the method for the heating is to be warming up to 300~500 DEG C with the rate of 2~5 DEG C/min, heat preservation
10~for 24 hours；The power of the laser irradiation is no more than 30W, and spot diameter is 10~15mm, and irradiation time is 5~20min.
Preferably, the method for the compacting be hydraulic method or isostatic pressing method, the hydraulic pressure be 2~
Between 15MPa, the compacting time is 3~10s；The pressure of the isostatic pressing method is 100~300MPa, and the compacting time is 3s.
Preferably, the illumination wavelength of laser described in step S2 is 980nm, and power is 90~1500W.
The present invention is applied to raw material using laser technology, by adjusting the input energy of laser, to control reaction process
Thermal barrier coating is grown on basis material, using laser technology with different adding material modes place selection containing rare earth element
Heat barrier coat material generates high-energy to be catalyzed reactant through laser irradiation, activated rare earth ion, and is allowed to and matrix surface
Thin layer melts simultaneously, and the coating that dilution is extremely low and matrix is in metallurgical bonding, the lasting confession of laser energy are quickly formed after solidification
The sensitization that stress send out rare earth ion more and multistep cascade reaction occurs, so that self- propagating grows thermal boundary such as layer on matrix,
Improve the performances such as wear-resisting, anti-corrosion, heat-resisting, anti-oxidant of substrate material surface.
The beneficial effects of the present invention are:
The various characteristics of prepared heat barrier coat material such as coating size, thickness, crystallinity, lattice types, lattice is big
It is small to be directly controlled by the power of adjusting laser, effect duration, the zone of action.Such technology has process flow letter
The features such as single, device is simple, and environmental requirement is not harsh, and synthesis cycle is short, and raw material availability is high, no coupling product.It is expected that can use
In industrial production large scale preparation high-performance heat barrier coat material.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is the reaction principle schematic diagram of thermal barrier coating prepared by embodiment 1 in the present invention；
Fig. 2 is that embodiment 1 prepares Er doping Yb in the present invention2Zr2O7The scanning electron microscope (SEM) photograph of thermal barrier coating；
Fig. 3 is to grow thermal barrier coating flow chart in the present invention involved in embodiment 2；
Fig. 4 is that embodiment 4 grows thermal barrier coating photo on stainless steel base in the present invention；
The thermal conductivity of Fig. 5 thermal barrier coating is tested.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
With rare earth Gd, the oxide Gd of Yb2O3、Yb2O3With the oxide ZrO of element Zr2According to molar ratio (Gd+
Yb): Zr=2:2, wherein the molar ratio of Gd and Yb is 1:4, calculates separately three kinds of oxide raw materials for weighing corrresponding quality, as
Raw material carry out high-energy ball milling mixing, and rotational speed of ball-mill 400rpm, Ball-milling Time 12h are full and uniform using acetone as ball milling medium
It is mixed to get raw mixture powder, the mix powder that ball milling is obtained is dried in 75 DEG C of baking ovens, ground, after grinding
Raw material be granulated grinding to obtain the product that microscopic particles are smaller, consistency is high, and granulation process is as follows: with PVA
Equal organic plastics are binder solute, and using deionized water as solvent, the binder that configuration quality score is 8% is divided to two to arrive
It is added in uniformly mixed powder three times, carries out grinding 3 hours, sieving, sieve mesh number is 30 mesh, and the powder after sieving is preset
In carrying out on matrix, laser pre-irradiation row is viscous, to remove bubble in coating.Then uniform fold is on alloy matrix aluminum, laser
Wavelength 980nm, laser sintered power 50W are irradiated or are sintered to the mixed-powder on alloy matrix aluminum, make raw mixture
Laser active self propagating high temperature solid phase reaction occurs, laser action time 5s obtains the Yb of Gd doping2Zr2O7Type ceramic with heat resistance applies
Layer.The coating is at 400 DEG C --- and thermal conductivity is reduced to 0.22W/mK from 1.04W/mK between 1000 DEG C.Fig. 1 is that growth thermal boundary applies
Layer schematic diagram, the growth Gd that Fig. 2 is adulterate Yb2Zr2O7The scanning electron microscope (SEM) photograph of thermal barrier coating.
Embodiment 2
With rare earth element er, the oxide Er of Yb2O3、Yb2O3With the oxide ZrO of element Zr2According to molar ratio (Er+
Yb): Zr=2:2, wherein the molar ratio of Er and Yb is 1:5, calculates separately three kinds of oxide raw materials for weighing corrresponding quality, as
Raw material progress high-energy ball milling mixing, rotational speed of ball-mill 400rpm, Ball-milling Time are for 24 hours, full and uniform using ethyl alcohol as ball milling medium
It is mixed to get raw mixture powder, the mix powder that ball milling is obtained is dried in 80 DEG C of baking ovens, ground, after grinding
Raw material be granulated grinding to obtain the product that microscopic particles are smaller, consistency is high, and granulation process is as follows: with PVA
Equal organic plastics are binder solute, and using deionized water as solvent, the binder that configuration quality score is 6% is divided to two to arrive
It is added in uniformly mixed powder three times, carries out grinding 4 hours, sieving, sieve mesh number is 50 mesh, and the powder after sieving is preset
In carrying out on matrix, laser pre-irradiation row is viscous, to remove bubble in coating.Then uniform fold is on alloy matrix aluminum, laser
Wavelength 980nm, laser sintered power 80W are irradiated or are sintered to the mixed-powder on alloy matrix aluminum, make raw mixture
Laser active self propagating high temperature solid phase reaction occurs, laser action time 10s obtains the Yb of Er doping2Zr2O7Type ceramic with heat resistance
Coating.The coating is at 400 DEG C --- and thermal conductivity is reduced to 0.80W/mK from 1.04W/mK between 800 DEG C.Fig. 3 is growth Er doping
Yb2Zr2O7Type thermal barrier coating flow chart.
Embodiment 3
With the oxide Yb of rare earth element y b2O3With the oxide ZrO of element Zr2According to molar ratio Yb:Zr=2:2, respectively
The two oxides raw material for weighing corrresponding quality is calculated, high-purity Si O is in addition weighed2Nano powder, quality are first two oxidation material
The 25% of amount, to prepare SiO2/Yb2Zr2O7Composite thermal barrier coating improves the corrosion resistance and heat-proof quality of thermal barrier coating, by three kinds
Oxide source materials carry out high-energy ball milling mixing, and using ethyl alcohol as ball milling medium, rotational speed of ball-mill 400rpm, the time is for 24 hours, full and uniform
It is mixed to get raw mixture powder, the mix powder that ball milling is obtained is dried in 80 DEG C of baking ovens, ground, after grinding
Raw material be granulated grinding to obtain the product that microscopic particles are smaller, consistency is high, and granulation process is as follows: with PVA
Equal organic plastics are binder solute, and using deionized water as solvent, the binder that configuration quality score is 6% is divided to two to arrive
It is added in uniformly mixed powder three times, carries out grinding 4 hours, sieving, sieve mesh number is 50 mesh, and the powder after sieving is preset
In carrying out on matrix, laser pre-irradiation row is viscous, to remove bubble in coating.Then uniform fold is on alloy matrix aluminum, laser
Wavelength 980nm, laser sintered power 80W are irradiated or are sintered to the mixed-powder on alloy matrix aluminum, make raw mixture
Laser active self propagating high temperature solid phase reaction occurs, laser action time 10s obtains SiO2/Yb2Zr2O7Composite thermal barrier coating.
The coating thermal conductivity test characterization such as Fig. 5.
Embodiment 4
With rare earth element er, the oxide Er of Yb2O3、Yb2O3With the oxide ZrO of element Zr2According to molar ratio (Er+
Yb): Zr=2:2, wherein the molar ratio of Er and Yb is 1:5, calculates separately three kinds of oxide raw materials for weighing corrresponding quality, as
Raw material progress high-energy ball milling mixing, rotational speed of ball-mill 400rpm, Ball-milling Time are for 24 hours, full and uniform using ethyl alcohol as ball milling medium
It is mixed to get raw mixture powder, the mix powder that ball milling is obtained is dried in 80 DEG C of baking ovens, ground, after grinding
Raw material progress is directly preset on stainless steel base, progress laser irradiation, and optical maser wavelength 980nm, laser sintered power 80W is right
Mixed-powder on stainless steel base is irradiated or is sintered, and makes raw mixture that laser active self propagating high temperature solid phase occur anti-
It answers, laser action time 10s, obtains the Yb of Er doping2Zr2O7Type heat barrier ceramic coating.Coating thermal conductivity at 1000 DEG C is
0.40W/mK.Fig. 4 is the growth thermal barrier coating photo on stainless steel base.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (8)
1. a kind of heat barrier coat material, which is characterized in that general molecular formula A2B2O7, wherein A Sc, Y, La, Nd, Eu, Gd,
At least one of Dy, Er, Yb and Lu, at least one of B Ti, Zr, Ce and Hf.
2. heat barrier coat material as described in claim 1, which is characterized in that molecular formula Yb2Zr2O7。
3. a kind of preparation method of heat barrier coat material as described in claim 1, which comprises the steps of:
S1, by oxide AOmWith oxide BOnAfter being mixed by underhand polish or ball milling, with dehydrated alcohol, acetone or deionization
Water is that medium carries out wet ball grinding, until partial size is no more than 1 μm, after product is taken out, drying, obtains abrasive material at 60~80 DEG C,
The abrasive material is ground, reaction powder is obtained；
S2, it after being compacted the reaction powder, is sintered under laser irradiation, obtains the ceramic electrolyte material；
Wherein, m and n is integer.
4. the preparation method of heat barrier coat material as claimed in claim 3, which is characterized in that further include to reaction in step S1
The step of powder is granulated, specifically:
The adhesive solution for being 1~10% by binder making mass fraction divides 2~3 times and is added in the reaction powder,
It ground, cross 20~50 meshes；
Include the steps that row is viscous in step S2, specifically:
Product after sieving is compacted, and it is viscous to carry out row by the method for heating or laser irradiation.
5. the preparation method of heat barrier coat material as claimed in claim 4, which is characterized in that the binder includes PVA, first
At least one of oxysilane, polyurethane, silicone.
6. the preparation method of heat barrier coat material as claimed in claim 4, which is characterized in that the method for the heating is, with 2~
The rate of 5 DEG C/min is warming up to 300~500 DEG C, and heat preservation 10~for 24 hours；The power of the laser irradiation is no more than 30W, and hot spot is straight
Diameter is 10~15mm, and irradiation time is 5~20min.
7. the preparation method of heat barrier coat material as claimed in claim 3, which is characterized in that the method for the compacting is hydraulic
Method or isostatic pressing method, for the hydraulic pressure between 2~15MPa, the compacting time is 3~10s；The pressure of the isostatic pressing method
For 100~300MPa, the compacting time is 3s.
8. the preparation method of heat barrier coat material as claimed in claim 3, which is characterized in that laser described in step S2
Illumination wavelength is 980nm, and power is 90~1500W.
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| CN201910696758.6A CN110256092A (en) | 2019-07-30 | 2019-07-30 | A kind of heat barrier coat material and preparation method thereof |
| US16/892,581 US11465911B2 (en) | 2019-07-30 | 2020-06-04 | Method for preparing ceramic material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112979310A (en) * | 2021-03-18 | 2021-06-18 | 中国科学院兰州化学物理研究所 | Aerospace thermal barrier material with low thermal conductivity and high fracture toughness and preparation thereof |
| CN114349502A (en) * | 2022-03-21 | 2022-04-15 | 中国人民解放军国防科技大学 | Titanium-doped lanthanum hafnate ceramic for low-thermal-expansion thermal/environmental barrier coating and preparation method thereof |
| CN116477940A (en) * | 2023-03-17 | 2023-07-25 | 电子科技大学 | Yttrium titanate doped zirconia ceramic material and preparation method and application thereof |
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| JPH06345568A (en) * | 1993-06-14 | 1994-12-20 | Nippon Pillar Packing Co Ltd | Production of coated material |
| CN1259588A (en) * | 1998-11-03 | 2000-07-12 | 大连理工大学 | Method of forming ceramic coating on metal surface by utilizing laser assisted self spreading |
| CN104630688A (en) * | 2015-01-23 | 2015-05-20 | 华中科技大学 | Method for preparing gradient thermal barrier coating |
| CN109851377A (en) * | 2019-03-18 | 2019-06-07 | 广东朗研科技有限公司 | A kind of induced with laser high temperature solid state reaction generation A2B2O7The method of type heat barrier coat material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06345568A (en) * | 1993-06-14 | 1994-12-20 | Nippon Pillar Packing Co Ltd | Production of coated material |
| CN1259588A (en) * | 1998-11-03 | 2000-07-12 | 大连理工大学 | Method of forming ceramic coating on metal surface by utilizing laser assisted self spreading |
| CN104630688A (en) * | 2015-01-23 | 2015-05-20 | 华中科技大学 | Method for preparing gradient thermal barrier coating |
| CN109851377A (en) * | 2019-03-18 | 2019-06-07 | 广东朗研科技有限公司 | A kind of induced with laser high temperature solid state reaction generation A2B2O7The method of type heat barrier coat material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112979310A (en) * | 2021-03-18 | 2021-06-18 | 中国科学院兰州化学物理研究所 | Aerospace thermal barrier material with low thermal conductivity and high fracture toughness and preparation thereof |
| CN114349502A (en) * | 2022-03-21 | 2022-04-15 | 中国人民解放军国防科技大学 | Titanium-doped lanthanum hafnate ceramic for low-thermal-expansion thermal/environmental barrier coating and preparation method thereof |
| CN114349502B (en) * | 2022-03-21 | 2022-06-03 | 中国人民解放军国防科技大学 | Titanium-doped lanthanum hafnate ceramic for low-thermal-expansion thermal/environmental barrier coating and preparation method thereof |
| CN116477940A (en) * | 2023-03-17 | 2023-07-25 | 电子科技大学 | Yttrium titanate doped zirconia ceramic material and preparation method and application thereof |
| CN116477940B (en) * | 2023-03-17 | 2024-04-12 | 电子科技大学 | Yttrium titanate doped zirconia ceramic material and preparation method and application thereof |
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