CN103113101A - Ceramic nano composite material for thermal barrier coating and preparation method thereof - Google Patents
Ceramic nano composite material for thermal barrier coating and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of a ceramic nano composite material and provides a ceramic nano composite material for a thermal barrier coating and a preparation method thereof. Cheap Ln(NO3)3.6H2O, Sr(NO3)2 and Zr(NO3)4.5H2O are used as raw materials, and the required ceramic nano composite material is obtained through solution preparation, burning and calcination. In the prepared ceramic nano composite material, the grain size of each phase is less than 70nm, and the phase distribution is uniform; and the ceramic nano composite material has good high-temperature chemical stability, anti-scouring property and heat insulation property, is favorable for suppressing the grain growth in high-temperature condition, improves the mechanical property (particularly toughness) of the ceramic nano composite material, and is a good candidate material serving as a thermal barrier coating. The preparation method of the ceramic nano composite material is simple, has the advantages of low synthesis temperature, short time and high phase purity, saves energy, is suitable for large-scale synthesis and has relatively great value in popularization and application.
Description
Technical field
The invention belongs to the ceramic nanocomposites technical field, relate in particular to a kind of ceramic nanocomposites for thermal barrier coating and preparation method thereof.
Background technology
Ceramic heat-barrier coating (ThermalBarrierCoatings, TBCs) be one of current state-of-the-art high-temperature protection coating, there are the characteristics such as good stability at elevated temperature, scour resistance and thermal insulation, can effectively alleviate high temperature oxidation and the corrosion of metal matrix material, and can reduce the working temperature of metal base surface, improve fuel economy, and can extend greatly life-span of turbine engine, in widespread attention and developed rapidly since early 1970s comes out.
In recent years, along with aero gas turbine engine, to high flow capacity ratio, high thrust-weight ratio, high inlet temperature future development, fuel gas temperature and pressure in combustion chamber also improve constantly.At present, the design temperature out of 10 grades of aircraft engines of thrust-weight ratio has reached more than 1577 ℃, and therefore, the alloy material surface of aero engine turbine blades needs ceramic coated thermal barrier coating to bear the turbine intake temperature more than 1600 ℃.The ZrO of 6wt.%-8wt.% stabilized with yttrium oxide
2(YSZ) be current most popular ceramic heat-barrier coating material.Because the life-time service temperature of YSZ can not be over 1200 ℃, along with temperature raises, phase transformation aggravates, easy-sintering, and the oxygen conductivity is high, and transition metal is easily oxidized, causes coating early failure, has been difficult to meet the further needs of raising turbine intake temperature.
Rare earth modified SrZrO
3characteristics with very high structural stability, lower thermal conductivity and anti-sintering are candidate material (W.Ma, D.Mack, J.Malzbender et al., the Yb of high-temp heat barrier coating
2o
3and Gd
2o
3doped strontium zirconate for thermal barrier coatings, J.Eur.Ceram.Soc.28 (16) (2008), pp.3071-3081).German patent DE 19801424 discloses and can, for the ceramic high-temperature insulation material more than 1000 ℃, be specially the La with pyrochlore constitution
2zr
2o
7with the BaZrO with perovskite structure
3with SrZrO
3.Rare earth zirconate (Ln
2zr
2o
7, Ln=La, Nd, Sm, Eu, Gd, Dy) and there is relatively low thermal conductivity and oxygen conductivity, but its thermal expansivity is relatively low, toughness is poor.Perovskite structure strontium zirconate (SrZrO
3) there is relatively high thermal expansivity and excellent stability at elevated temperature, but its thermal conductivity is relatively high, toughness is poor.
At present, the preparation method of above-mentioned materials is mainly high-temperature solid phase reaction method.Adopt SrCO
3, Ln
2o
3(Ln=La, Nd, Sm, Eu, Gd, Dy) and ZrO
2for raw material, synthetic through ball milling, oven dry, calcining, calcining temperature is usually more than 1400 ℃, and calcination time is long, need to repeatedly repeat said process and just can obtain material requested, length consuming time, consume energy high.
Summary of the invention
The invention provides a kind of ceramic nanocomposites for thermal barrier coating and preparation method thereof, be intended to solve the material as ceramic heat-barrier coating that prior art provides, the performance that stability at elevated temperature, thermal conductivity are relatively low, toughness is higher that can not simultaneously possess higher thermal expansivity, excellence, be difficult to meet the needs that further improve turbine intake temperature, and calcination time is long while preparing above-mentioned materials, preparation process is complicated, length consuming time, high problem consumes energy.
The object of the present invention is to provide a kind of ceramic nanocomposites for thermal barrier coating, the chemical constitution of this ceramic nanocomposites is (Sr
1-xln
x) ZrO
3+ δ;
Wherein, 0.1≤x≤0.9, Ln is one or more the combination in La, Nd, Sm, Eu, Gd, Dy.
Further, in described ceramic nanocomposites, the grain-size of each phase all is less than 70nm.
Further, described ceramic nanocomposites can be: (Sr
0.9la
0.1) ZrO
3.05, (Sr
0.6sm
0.4) ZrO
3.2, (Sr
0.4eu
0.6) ZrO
3.3, (Sr
0.4gd
0.6) ZrO
3.3, (Sr
0.1dy
0.9) ZrO
3.45, (Sr
0.6nd
0.4) ZrO
3.2, (Sr
0.7gd
0.3) ZrO
3.15, (Sr
0.5gd
0.5) ZrO
3.25, (Sr
0.3gd
0.7) ZrO
3.35, (Sr
0.7la
0.3) ZrO
3.15, (Sr
0.5la
0.5) ZrO
3.25, (Sr
0.3la
0.7) ZrO
3.35, (Sr
0.7nd
0.3) ZrO
3.15, (Sr
0.5nd
0.5) ZrO
3.25, (Sr
0.3nd
0.7) ZrO
3.35, (Sr
0.7sm
0.3) ZrO
3.15, (Sr
0.5sm
0.5) ZrO
3.25, (Sr
0.3sm
0.7) ZrO
3.35, (Sr
0.7eu
0.3) ZrO
3.15, (Sr
0.5eu
0.5) ZrO
3.25, (Sr
0.3eu
0.7) ZrO
3.35, (Sr
0.7dy
0.3) ZrO
3.15, (Sr
0.5dy
0.5) ZrO
3.25, (Sr
0.3dy
0.7) ZrO
3.35in any one.
Further, described ceramic nanocomposites also can be: (Sr
0.9(LaNd)
0.1) ZrO
3.05, (Sr
0.8(LaSm)
0.2) ZrO
3.1, (Sr
0.7(LaEu)
0.3) ZrO
3.15, (Sr
0.6(LaGd)
0.4) ZrO
3.2, (Sr
0.5(LaDy)
0.5) ZrO
3.25, (Sr
0.4(NdSm)
0.6) ZrO
3.3, (Sr
0.3(NdEu)
0.7) ZrO
3.35, (Sr
0.2(NdGd)
0.8) ZrO
3.4, (Sr
0.1(NdDy)
0.9) ZrO
3.45, (Sr
0.8(SmEu)
0.2) ZrO
3.1, (Sr
0.7(SmGd)
0.3) ZrO
3.15, (Sr
0.6(SmDy)
0.4) ZrO
3.2, (Sr
0.5(EuGd)
0.5) ZrO
3.25, (Sr
0.4(EuDy)
0.6) ZrO
3.3, (Sr
0.3(GdDy)
0.7) ZrO
3.35in any one.
Another object of the present invention is to provide a kind of preparation method of the ceramic nanocomposites for thermal barrier coating, this preparation method comprises the following steps:
With Sr (NO
3)
2, Ln (NO
3)
36H
2o and Zr (NO
3)
45H
2o is raw material, by (1-x): the x:1 mixed in molar ratio, 0.1≤x≤0.9 wherein, Ln is one or more the combination in La, Nd, Sm, Eu, Gd, Dy;
Take distilled water as solvent, and dehydrated alcohol is ignition dope, adds appropriate citric acid and polyoxyethylene glycol, and magnetic agitation is to the solution of clear;
The solution made is put into to the ignition of zirconium white crucible, obtain the required presoma of sample;
The presoma obtained is carried out to high-temperature calcination.
Further, to belong to ionic concn be 0.05-0.7mol/L to described GOLD FROM PLATING SOLUTION.
Further, in described solution the mol ratio of positively charged ion and citric acid between 1:1 to 1:2.
Further, the implementation method that the described presoma to acquisition carries out high-temperature calcination is:
By program control High Temperature Furnaces Heating Apparatus, presoma is warmed up to 1000 ℃-1400 ℃ with 5-10 ℃/min speed;
Presoma is incubated to 2 to 6h.
Ceramic nanocomposites for thermal barrier coating provided by the invention and preparation method thereof, used cheap Ln (NO
3)
36H
2o, Sr (NO
3)
2and Zr (NO
3)
45H
2o is raw material, through solution, prepare, burning, calcining, obtain required ceramic nanocomposites, in prepared ceramic nanocomposites, each phase grain-size all is less than 70nm, and distribution of each phase is even, there is good stability at elevated temperature, scour resistance and thermal insulation, be conducive to suppress grain growth under hot conditions, and the mechanical property of raising ceramic nanocomposites itself, toughness particularly, it is the good candidate material as thermal barrier coating, the preparation method is simple for this ceramic nanocomposites, synthesis temperature is relatively low, time is short, phase purity is high, save energy, be applicable to a large amount of synthetic, there is stronger popularization and using value.
The accompanying drawing explanation
Fig. 1 is the preparation method's of the ceramic nanocomposites for thermal barrier coating that provides of the embodiment of the present invention realization flow figure;
Fig. 2 is the schema that the presoma to obtaining that the embodiment of the present invention provides carries out the implementation method of high-temperature calcination;
Fig. 3 is the XRD figure spectrum of the ceramic nanocomposites that provides of the embodiment of the present invention;
Fig. 4 is the TEM photo of the ceramic nanocomposites that provides of the embodiment of the present invention.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is described in further detail.Should be appreciated that specific embodiment described herein is only in order to explain the present invention, and be not used in the restriction invention.
The object of the present invention is to provide a kind of ceramic nanocomposites for thermal barrier coating, the chemical constitution of this ceramic nanocomposites is (Sr
1-xln
x) ZrO
3+ δ;
Wherein, 0.1≤x≤0.9, Ln is one or more the combination in La, Nd, Sm, Eu, Gd, Dy.
In embodiments of the present invention, in this ceramic nanocomposites, the grain-size of each phase all is less than 70nm.
In embodiments of the present invention, this ceramic nanocomposites can be:
(Sr
0.9la
0.1) ZrO
3.05or (Sr
0.6sm
0.4) ZrO
3.2or (Sr
0.4eu
0.6) ZrO
3.3or (Sr
0.4gd
0.6) ZrO
3.3or (Sr
0.1dy
0.9) ZrO
3.45or (Sr
0.6nd
0.4) ZrO
3.2or (Sr
0.7gd
0.3) ZrO
3.15or (Sr
0.5gd
0.5) ZrO
3.25or (Sr
0.3gd
0.7) ZrO
3.35or (Sr
0.7la
0.3) ZrO
3.15or (Sr
0.5la
0.5) ZrO
3.25or (Sr
0.3la
0.7) ZrO
3.35or (Sr
0.7nd
0.3) ZrO
3.15or (Sr
0.5nd
0.5) ZrO
3.25or (Sr
0.3nd
0.7) ZrO
3.35or (Sr
0.7sm
0.3) ZrO
3.15or (Sr
0.5sm
0.5) ZrO
3.25or (Sr
0.3sm
0.7) ZrO
3.35or (Sr
0.7eu
0.3) ZrO
3.15or (Sr
0.5eu
0.5) ZrO
3.25or (Sr
0.3eu
0.7) ZrO
3.35or (Sr
0.7dy
0.3) ZrO
3.15or (Sr
0.5dy
0.5) ZrO
3.25or (Sr
0.3dy
0.7) ZrO
3.35.
In embodiments of the present invention, this ceramic nanocomposites also can be:
(Sr
0.9(LaNd)
0.1) ZrO
3.05or (Sr
0.8(LaSm)
0.2) ZrO
3.1or (Sr
0.7(LaEu)
0.3) ZrO
3.15or (Sr
0.6(LaGd)
0.4) ZrO
3.2or (Sr
0.5(LaDy)
0.5) ZrO
3.25or (Sr
0.4(NdSm)
0.6) ZrO
3.3or (Sr
0.3(NdEu)
0.7) ZrO
3.35or (Sr
0.2(NdGd)
0.8) ZrO
3.4or (Sr
0.1(NdDy)
0.9) ZrO
3.45or (Sr
0.8(SmEu)
0.2) ZrO
3.1or (Sr
0.7(SmGd)
0.3) ZrO
3.15or (Sr
0.6(SmDy)
0.4) ZrO
3.2or (Sr
0.5(EuGd)
0.5) ZrO
3.25or (Sr
0.4(EuDy)
0.6) ZrO
3.3or (Sr
0.3(GdDy)
0.7) ZrO
3.35.
Fig. 3 is the XRD figure spectrum of ceramic nanocomposites, shows that this ceramic nanocomposites is SrZrO
3and La
2zr
2o
7matrix material.
Fig. 4 is the TEM photo of ceramic nanocomposites, shows that this ceramic nanocomposites is nano level matrix material, and grain size is between 30-50nm.
Fig. 1 shows the preparation method's of the ceramic nanocomposites for thermal barrier coating that the embodiment of the present invention provides realization flow.
This preparation method comprises the following steps:
In step S101, with Sr (NO
3)
2, Ln (NO
3)
36H
2o and Zr (NO
3)
45H
2o is raw material, by (1-x): the x:1 mixed in molar ratio, 0.1≤x≤0.9 wherein, Ln is one or more the combination in La, Nd, Sm, Eu, Gd, Dy;
In step S102, take distilled water as solvent, dehydrated alcohol is ignition dope, adds appropriate citric acid and polyoxyethylene glycol, magnetic agitation is to the solution of clear;
In step S103, the solution made is put into to the ignition of zirconium white crucible, obtain the required presoma of sample;
In step S104, the presoma obtained is carried out to high-temperature calcination.
In embodiments of the present invention, to belong to ionic concn be 0.05-0.7mol/L to GOLD FROM PLATING SOLUTION.
In embodiments of the present invention, in solution the mol ratio of positively charged ion and citric acid between 1:1 to 1:2.
As shown in Figure 2, in embodiments of the present invention, the implementation method of the presoma obtained being carried out to high-temperature calcination is:
In step S201, by program control High Temperature Furnaces Heating Apparatus, presoma is warmed up to 1000 ℃-1400 ℃ with 5-10 ℃/min speed;
In step S202, presoma is incubated to 2 to 6h.
Below in conjunction with drawings and the specific embodiments, application principle of the present invention is further described.
One of purpose of the embodiment of the present invention is to provide a kind of ceramic nanocomposites for thermal barrier coating, and the chemical constitution of this ceramic nanocomposites is (Sr
1-xln
x) ZrO
3+ δ, 0.1≤x≤0.9, Ln is one or more combination in La, Nd, Sm, Eu, Gd, Dy.
This ceramic nanocomposites has: (Sr
0.9la
0.1) ZrO
3.05or (Sr
0.6sm
0.4) ZrO
3.2or (Sr
0.4eu
0.6) ZrO
3.3or (Sr
0.4gd
0.6) ZrO
3.3or (Sr
0.1dy
0.9) ZrO
3.45or (Sr
0.6nd
0.4) ZrO
3.2or (Sr
0.7gd
0.3) ZrO
3.15or (Sr
0.5gd
0.5) ZrO
3.25or (Sr
0.3gd
0.7) ZrO
3.35or (Sr
0.7la
0.3) ZrO
3.15or (Sr
0.5la
0.5) ZrO
3.25or (Sr
0.3la
0.7) ZrO
3.35or (Sr
0.7nd
0.3) ZrO
3.15or (Sr
0.5nd
0.5) ZrO
3.25or (Sr
0.3nd
0.7) ZrO
3.35or (Sr
0.7sm
0.3) ZrO
3.15or (Sr
0.5sm
0.5) ZrO
3.25or (Sr
0.3sm
0.7) ZrO
3.35or (Sr
0.7eu
0.3) ZrO
3.15or (Sr
0.5eu
0.5) ZrO
3.25or (Sr
0.3eu
0.7) ZrO
3.35or (Sr
0.7dy
0.3) ZrO
3.15or (Sr
0.5dy
0.5) ZrO
3.25or (Sr
0.3dy
0.7) ZrO
3.35;
This ceramic nanocomposites also has: (Sr
0.9(LaNd)
0.1) ZrO
3.05or (Sr
0.8(LaSm)
0.2) ZrO
3.1or (Sr
0.7(LaEu)
0.3) ZrO
3.15or (Sr
0.6(LaGd)
0.4) ZrO
3.2or (Sr
0.5(LaDy)
0.5) ZrO
3.25or (Sr
0.4(NdSm)
0.6) ZrO
3.3or (Sr
0.3(NdEu)
0.7) ZrO
3.35or (Sr
0.2(NdGd)
0.8) ZrO
3.4or (Sr
0.1(NdDy)
0.9) ZrO
3.45or (Sr
0.8(SmEu)
0.2) ZrO
3.1or (Sr
0.7(SmGd)
0.3) ZrO
3.15or (Sr
0.6(SmDy)
0.4) ZrO
3.2or (Sr
0.5(EuGd)
0.5) ZrO
3.25or (Sr
0.4(EuDy)
0.6) ZrO
3.3or (Sr
0.3(GdDy)
0.7) ZrO
3.35.
As shown in Figure 1, another purpose of the embodiment of the present invention is to provide a kind of preparation method of the ceramic nanocomposites for thermal barrier coating, and its preparation process is as follows:
With Sr (NO
3)
2, Ln (NO
3)
36H
2o and Zr (NO
3)
45H
2o is raw material, by (1-x): the x:1 mixed in molar ratio, 0.1≤x≤0.9, Ln is one or more combination in La, Nd, Sm, Eu, Gd, Dy;
Take distilled water as solvent, and dehydrated alcohol is ignition dope, adds appropriate citric acid and polyoxyethylene glycol, and magnetic agitation is to the solution of clear;
The solution made is put into to the ignition of zirconium white crucible, obtain the required presoma of sample;
Presoma is put into to 1000 ℃-1400 ℃ calcining 2-6h of program control High Temperature Furnaces Heating Apparatus, can obtain required ceramic nanocomposites.
Embodiment 1:
Preparation nano composite material (Sr
0.5la
0.5) ZrO
3.25, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: La (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.5:0.5:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.5mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 21.014g, additional PEG 20000 is additive, and addition is 5g, then adds dehydrated alcohol, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1200 ℃, calcine 5h, then can obtain required nano composite material with the stove cooling.Fig. 3 is the XRD figure spectrum of synthetic materials, shows that synthetic material is SrZrO
3and La
2zr
2o
7matrix material.Fig. 4 is the TEM photo of synthetic materials, shows that this matrix material is nano level matrix material, and grain size is between 30-50nm.
Embodiment 2:
Prepare nano composite material (Sr by the method for embodiment 1
0.3la
0.7) ZrO
3.35, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: La (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.3:0.7:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.05mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 2.10g, additional PEG 20000 is additive, and addition is 5g, then adds dehydrated alcohol, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1000 ℃, calcine 4h, then can obtain required nano composite material with the stove cooling.
Embodiment 3:
Prepare nano composite material (Sr by the method for embodiment 1
0.7la
0.3) ZrO
3.15, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: La (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.7:0.3:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.06mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 2.42g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1100 ℃, calcine 2h, then can obtain required nano composite material with the stove cooling.
Embodiment 4:
Prepare nano composite material (Sr by the method for embodiment 1
0.9la
0.1) ZrO
3.05, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: La (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.9:0.1:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.07mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 2.94g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1100 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 5:
Prepare nano composite material (Sr by the method for embodiment 1
0.4gd
0.6) ZrO
3.3, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Gd (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.4:0.6:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.08mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 3.36g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1200 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 6:
Prepare nano composite material (Sr by embodiment 1 method
0.3gd
0.7) ZrO
3.35, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Gd (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.3:0.7:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.09mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 3.56g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1100 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 7:
Prepare nano composite material (Sr by embodiment 1 method
0.5gd
0.5) ZrO
3.25, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Gd (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.5:0.5:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.10mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 4.10g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1200 ℃, calcine 4h, then can obtain required nano composite material with the stove cooling.
Embodiment 8:
Prepare nano composite material (Sr by embodiment 1 method
0.7gd
0.3) ZrO
3.15, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Gd (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.7:0.3:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.11mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 4.32g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1200 ℃, calcine 4h, then can obtain required nano composite material with the stove cooling.
Embodiment 9:
Prepare nano composite material (Sr by embodiment 1 method
0.6nd
0.4) ZrO
3.2, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Nd (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.6:0.4:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.12mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 4.45g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1100 ℃, calcine 5h, then can obtain required nano composite material with the stove cooling.
Embodiment 10:
Prepare nano composite material (Sr by embodiment 1 method
0.3nd
0.7) ZrO
3.35, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Nd (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.3:0.7:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.13mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 4.84g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1200 ℃, calcine 2h, then can obtain required nano composite material with the stove cooling.
Embodiment 11:
Prepare nano composite material (Sr by embodiment 1 method
0.5nd
0.5) ZrO
3.25, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Nd (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.5:0.5:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.14mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 5.56g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1100 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 12:
Prepare nano composite material (Sr by embodiment 1 method
0.7nd
0.3) ZrO
3.15, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Nd (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.7:0.3:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.16mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 6.24g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1100 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 13:
Prepare nano composite material (Sr by embodiment 1 method
0.6sm
0.4) ZrO
3.2, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Sm (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.6:0.4:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.20mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 8.33g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1200 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 14:
Prepare nano composite material (Sr by embodiment 1 method
0.3sm
0.7) ZrO
3.35, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Sm (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.3:0.7:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.24mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 8.96g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1300 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 15:
Prepare nano composite material (Sr by embodiment 1 method
0.5sm
0.5) ZrO
3.25, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Sm (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.5:0.5:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.26mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 9.50g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1300 ℃, calcine 4h, then can obtain required nano composite material with the stove cooling.
Embodiment 16:
Prepare nano composite material (Sr by embodiment 1 method
0.7sm
0.3) ZrO
3.15, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Sm (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.7:0.3:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.28mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 9.98g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1300 ℃, calcine 4h, then can obtain required nano composite material with the stove cooling.
Embodiment 17:
Prepare nano composite material (Sr by embodiment 1 method
0.4eu
0.6) ZrO
3.3, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Eu (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.4:0.6:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.30mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 10.58g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1300 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 18:
Prepare nano composite material (Sr by embodiment 1 method
0.3eu
0.7) ZrO
3.35, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Eu (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.3:0.7:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.32mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 11.87g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1300 ℃, calcine 4h, then can obtain required nano composite material with the stove cooling.
Embodiment 19:
Prepare nano composite material (Sr by embodiment 1 method
0.5eu
0.5) ZrO
3.25, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Eu (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.5:0.5:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.36mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 12.24g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1300 ℃, calcine 4h, then can obtain required nano composite material with the stove cooling.
Embodiment 20:
Prepare nano composite material (Sr by embodiment 1 method
0.7eu
0.3) ZrO
3.15, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Eu (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.7:0.3:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.38mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 13.36g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1300 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 21:
Prepare nano composite material (Sr by embodiment 1 method
0.1dy
0.9) ZrO
3.45, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Dy (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.1:0.9:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.40mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 15.46g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1200 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 22:
Prepare nano composite material (Sr by embodiment 1 method
0.3dy
0.7) ZrO
3.35, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Dy (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.3:0.7:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.42mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 16.56g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1400 ℃, calcine 2h, then can obtain required nano composite material with the stove cooling.
Embodiment 23:
With embodiment 1 method preparation (Sr
0.5dy
0.5) ZrO
3.25, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Dy (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.5:0.5:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.44mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 17.44g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1400 ℃, calcine 3h, then can obtain required nano composite material with the stove cooling.
Embodiment 24:
With embodiment 1 method preparation (Sr
0.7dy
0.3) ZrO
3.15, raw material is pressed following proportioning (mol ratio): Sr (NO
3)
2: Dy (NO
3)
36H
2o:Zr (NO
3)
45H
2the O=0.7:0.3:1 accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.58mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 19.66g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1400 ℃, calcine 5h, then can obtain required nano composite material with the stove cooling.
Embodiment 25:
Prepare following nano composite material by embodiment 1 method: (Sr
0.9(LaNd)
0.1) ZrO
3.05or (Sr
0.8(LaSm)
0.2) ZrO
3.1or (Sr
0.7(LaEu)
0.3) ZrO
3.15or (Sr
0.6(LaGd)
0.4) ZrO
3.2or (Sr
0.5(LaDy)
0.5) ZrO
3.25or (Sr
0.4(NdSm)
0.6) ZrO
3.3or (Sr
0.3(NdEu)
0.7) ZrO
3.35or (Sr
0.2(NdGd)
0.8) ZrO
3.4or (Sr
0.1(NdDy)
0.9) ZrO
3.45or (Sr
0.8(SmEu)
0.2) ZrO
3.1or (Sr
0.7(SmGd)
0.3) ZrO
3.15or (Sr
0.6(SmDy)
0.4) ZrO
3.2or (Sr
0.5(EuGd)
0.5) ZrO
3.25or (Sr
0.4(EuDy)
0.6) ZrO
3.3or (Sr
0.3(GdDy)
0.7) ZrO
3.35;
Raw material is by its proportioning (mol ratio) accurate measuring, take distilled water as solvent, the solution 100ml that to prepare total strength of solution be 0.6mol/L, and be placed on magnetic stirrer and stir raw material is fully dissolved, outer adding citric acid is complexing agent, addition is 22.56g, additional PEG 20000 is additive, and addition is 5g, then to add dehydrated alcohol be ignition dope, addition is 300ml, continues to stir to make it clear.The solution of acquisition is put into to the zirconium white crucible, and ignition, obtain the presoma of required sample, presoma put into to retort furnace and under 1400 ℃, calcine 5h, then can obtain required nano composite material with the stove cooling.
Ceramic nanocomposites for thermal barrier coating that the embodiment of the present invention provides and preparation method thereof, used cheap Ln (NO
3)
36H
2o, Sr (NO
3)
2and Zr (NO
3)
45H
2o is raw material, through solution, prepare, burning, calcining, obtain required ceramic nanocomposites, in prepared ceramic nanocomposites, each phase grain-size all is less than 70nm, and distribution of each phase is even, there is good stability at elevated temperature, scour resistance and thermal insulation, be conducive to suppress grain growth under hot conditions, and the mechanical property of raising ceramic nanocomposites itself, toughness particularly, it is the good candidate material as thermal barrier coating, the preparation method is simple for this ceramic nanocomposites, synthesis temperature is relatively low, time is short, phase purity is high, save energy, be applicable to a large amount of synthetic, there is stronger popularization and using value.
These are only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. the ceramic nanocomposites for thermal barrier coating, is characterized in that, the chemical constitution of this ceramic nanocomposites is (Sr
1-xln
x) ZrO
3+ δ; Wherein, 0.1≤x≤0.9, Ln is one or more the combination in La, Nd, Sm, Eu, Gd, Dy.
2. ceramic nanocomposites as claimed in claim 1, is characterized in that, in described ceramic nanocomposites, the grain-size of each phase all is less than 70nm.
3. ceramic nanocomposites as claimed in claim 1, is characterized in that, described ceramic nanocomposites can be: (Sr
0.9la
0.1) ZrO
3.05, (Sr
0.6sm
0.4) ZrO
3.2, (Sr
0.4eu
0.6) ZrO
3.3, (Sr
0.4gd
0.6) ZrO
3.3, (Sr
0.1dy
0.9) ZrO
3.45, (Sr
0.6nd
0.4) ZrO
3.2, (Sr
0.7gd
0.3) ZrO
3.15, (Sr
0.5gd
0.5) ZrO
3.25, (Sr
0.3gd
0.7) ZrO
3.35, (Sr
0.7la
0.3) ZrO
3.15, (Sr
0.5la
0.5) ZrO
3.25, (Sr
0.3la
0.7) ZrO
3.35, (Sr
0.7nd
0.3) ZrO
3.15, (Sr
0.5nd
0.5) ZrO
3.25, (Sr
0.3nd
0.7) ZrO
3.35, (Sr
0.7sm
0.3) ZrO
3.15, (Sr
0.5sm
0.5) ZrO
3.25, (Sr
0.3sm
0.7) ZrO
3.35, (Sr
0.7eu
0.3) ZrO
3.15, (Sr
0.5eu
0.5) ZrO
3.25, (Sr
0.3eu
0.7) ZrO
3.35, (Sr
0.7dy
0.3) ZrO
3.15, (Sr
0.5dy
0.5) ZrO
3.25, (Sr
0.3dy
0.7) ZrO
3.35in any one.
4. ceramic nanocomposites as described as claim 1 or 3, is characterized in that, described ceramic nanocomposites also can be: (Sr
0.9(LaNd)
0.1) ZrO
3.05, (Sr
0.8(LaSm)
0.2) ZrO
3.1, (Sr
0.7(LaEu)
0.3) ZrO
3.15, (Sr
0.6(LaGd)
0.4) ZrO
3.2, (Sr
0.5(LaDy)
0.5) ZrO
3.25, (Sr
0.4(NdSm)
0.6) ZrO
3.3, (Sr
0.3(NdEu)
0.7) ZrO
3.35, (Sr
0.2(NdGd)
0.8) ZrO
3.4, (Sr
0.1(NdDy)
0.9) ZrO
3.45, (Sr
0.8(SmEu)
0.2) ZrO
3.1, (Sr
0.7(SmGd)
0.3) ZrO
3.15, (Sr
0.6(SmDy)
0.4) ZrO
3.2, (Sr
0.5(EuGd)
0.5) ZrO
3.25, (Sr
0.4(EuDy)
0.6) ZrO
3.3, (Sr
0.3(GdDy)
0.7) ZrO
3.35in any one.
5. the preparation method for the ceramic nanocomposites of thermal barrier coating, is characterized in that, this preparation method comprises the following steps:
With Sr (NO
3)
2, Ln (NO
3)
36H
2o and Zr (NO
3)
45H
2o is raw material, by (1-x): the x:1 mixed in molar ratio, 0.1≤x≤0.9 wherein, Ln is one or more the combination in La, Nd, Sm, Eu, Gd, Dy;
Take distilled water as solvent, and dehydrated alcohol is ignition dope, adds appropriate citric acid and polyoxyethylene glycol, and magnetic agitation is to the solution of clear;
The solution made is put into to the ignition of zirconium white crucible, obtain the required presoma of sample;
The presoma obtained is carried out to high-temperature calcination.
6. preparation method according to claim 5, is characterized in that, it is 0.05-0.7mol/L that described GOLD FROM PLATING SOLUTION belongs to ionic concn.
7. according to the described preparation method of claim 5 or 6, it is characterized in that, in described solution, the mol ratio of positively charged ion and citric acid is between 1:1 to 1:2.
8. preparation method according to claim 5, is characterized in that, the implementation method that the described presoma to acquisition carries out high-temperature calcination is:
By program control High Temperature Furnaces Heating Apparatus, presoma is warmed up to 1000 ℃-1400 ℃ with 5-10 ℃/min speed;
Presoma is incubated to 2 to 6h.
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CN103285850A (en) * | 2013-06-28 | 2013-09-11 | 河南省格林沃特净化器股份有限公司 | Method for preparing lanthanum-cerium-zirconium complex through atomization combustion |
CN104803677A (en) * | 2014-07-28 | 2015-07-29 | 内蒙古英诺威科技有限公司 | Thermal barrier coating material, thermal barrier coating and preparation method thereof |
CN110803924A (en) * | 2019-12-03 | 2020-02-18 | 内蒙古工业大学 | Strontium zirconate-based composite ceramic thermal barrier coating material with low thermal conductivity and high phase stability as well as preparation method and application thereof |
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CN101948995A (en) * | 2010-09-27 | 2011-01-19 | 内蒙古工业大学 | Ceramic composite thermal barrier coating material |
CN102030368A (en) * | 2010-11-18 | 2011-04-27 | 西南科技大学 | Preparation method of pure-phase high-performance rare earth zirconate material |
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2013
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CN101948995A (en) * | 2010-09-27 | 2011-01-19 | 内蒙古工业大学 | Ceramic composite thermal barrier coating material |
CN102030368A (en) * | 2010-11-18 | 2011-04-27 | 西南科技大学 | Preparation method of pure-phase high-performance rare earth zirconate material |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103285850A (en) * | 2013-06-28 | 2013-09-11 | 河南省格林沃特净化器股份有限公司 | Method for preparing lanthanum-cerium-zirconium complex through atomization combustion |
CN103285850B (en) * | 2013-06-28 | 2015-04-22 | 河南省格林沃特净化器股份有限公司 | Method for preparing lanthanum-cerium-zirconium complex through atomization combustion |
CN104803677A (en) * | 2014-07-28 | 2015-07-29 | 内蒙古英诺威科技有限公司 | Thermal barrier coating material, thermal barrier coating and preparation method thereof |
CN110803924A (en) * | 2019-12-03 | 2020-02-18 | 内蒙古工业大学 | Strontium zirconate-based composite ceramic thermal barrier coating material with low thermal conductivity and high phase stability as well as preparation method and application thereof |
CN110803924B (en) * | 2019-12-03 | 2022-03-04 | 内蒙古工业大学 | Strontium zirconate-based composite ceramic thermal barrier coating material with low thermal conductivity and high phase stability as well as preparation method and application thereof |
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