CN104988455B - A kind of air plasma spraying preparation method of the heat-barrier coating ceramic layer of anti-CMAS corrosion - Google Patents
A kind of air plasma spraying preparation method of the heat-barrier coating ceramic layer of anti-CMAS corrosion Download PDFInfo
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Abstract
The invention discloses a kind of air plasma spraying preparation methods of the heat-barrier coating ceramic layer of anti-CMAS corrosion, belong to heat barrier coat material and its preparation field.The present invention prepares one layer of second ceramic layer using air plasma spraying method on YSZ ceramic layers, second ceramic layer is poor to the wetability for melting CMAS, after 1250 DEG C of heat treatments, one layer of mutual reactance layer is formed in the second ceramic layer and the interfaces CMAS, penetrating further into for melting CMAS is effectively prevented, YSZ ceramic layers maintain original phase stability.Therefore, the second ceramic layer that prepared by the present invention can prevent the infiltration of melting CMAS, and the performance that there is excellent anti-CMAS to corrode significantly improves the service life of thermal barrier coating under CMAS couplings.
Description
Technical field
The present invention relates to thermal barrier coating preparing technical fields, more specifically refer to preparing one using air plasma spraying method
The heat-barrier coating ceramic layer of the anti-CMAS corrosion of kind.
Background technology
Thermal barrier coating (Thermal Barrier Coatings), abbreviation TBCs is advanced aero engine hot-end component
One of crucial science and technology.The study found that aero engine turbine blades thermal barrier coating in addition to high temperature to be subjected to, heat fatigue and
Outside the effects that mechanical load, chemical attack is may also suffer, corrodes and washes away, eventually leads to coating failure.Wherein, by calcium oxide
(CaO), magnesia (MgO), alundum (Al2O3) (Al2O3), silica (SiO2) and trace vanadium, sulphur, sodium, ferro element composition
Surface deposits (CMAS) it is very big to the heat-proof quality of TBCs and the influence of service life.
Current most widely used heat-barrier coating ceramic layer material is yttrium partially stabilized zirconium oxide (YSZ, the ZrO of oxidation2+
(6~8wt%) Y2O3), but in 1250 DEG C and higher temperature, there are significant destructions to YSZ ceramic layers by CMAS, mainly
It shows：Melting CMAS penetrates into coat inside by the gap and crackle of YSZ surface ceramii layers, shock compaction YSZ ceramic layers,
And larger internal stress is generated, lead to the layering of YSZ ceramic layers, peel off；YSZ ceramic layers are gradually melted in glassy state CMAS, are made
At stabilizer yttrium oxide (Y2O3) loss, zirconium oxide (ZrO2) crystal transfer occurs, reduce coating strain Damage tolerance；CMAS
The interior diffusion of middle Si, Ca exacerbate the sintering of YSZ ceramic layers, considerably reduce porosity, and the heat-insulating capability of TBCs drastically declines.
The main method for preparing anti-CMAS protective coatings has：Magnetron sputtering, EB-PVD, APS, electrophoretic deposition, CVD, coating
Be heat-treated after powder, solution infiltration and fuse salt coating etc..(see reference Aygun A. etc. document 1：Aygun A,Vasiliev
Al L,Padture N P,Ma X Q.Acta Material 2007,55:6734-45.) the study found that using SPPS methods
Alundum (Al2O3) (the Al of (molar percentage) 20% is added in YSZ2O3) and (molar percentage) 5% titanium dioxide
(TiO2) YSZ+Al+Ti layers are formed, as modified YSZ ceramic layers, TiO2To melt the nucleating agent of CMAS, Al2O3Promote melting
CMAS is crystallized, and to make melting CMAS in modified YSZ surface ceramii layers crystallization, is hindered in the case where not influencing TBCs uses
Stopped the infiltration of CMAS, but YSZ is in the sintering phenomenon for being easy to happen phase transformation and zirconium oxide higher than 1200 DEG C, make its application by
Limitation.Mohan P. etc. use electrophoresis in YSZ surface ceramii layer deposition of aluminium oxide, then are sintered, and obtain fine and close protection
Layer, and then (see reference document 2 for the infiltration of prevention melting CMAS：Mohan P,Yao B,Patterson T,Sohn Y
H.Surface&Coatings Technology 2009,204:797–801).Alumina layer and YSZ ceramic layer coefficient of thermal expansion
It mismatches so that service life of the TBCs coatings in thermal cycle experiment is relatively low, limits the application of the method.
Invention content
The object of the present invention is to provide a kind of preparation methods of the heat-barrier coating ceramic layer of anti-CMAS corrosion, more specifically refer to and answer
With air plasma spraying (APS) method in YSZ ceramic layers one layer of second ceramic layer prepared above.Second ceramic layer is in synusia
Shape, compact structure, thermal conductivity is low, and high temperature phase stability is good.The second ceramic layer of surface coating CMAS is heat-treated 30h at 1250 DEG C
Afterwards, one layer of mutual reactance layer is formed at the interface of CMAS layers and the second ceramic layer, the main component of mutual reactance layer is La and Ca, Si shape
At a kind of high-melting-point, high-compactness open structure silicate oxyapatite phase, mutual reactance layer effectively prevents molten
Melt the infiltration of CMAS, i.e., effectively prevents further infringement of Ca, Si element to thermal barrier coating.
A kind of air plasma spraying preparation method of the heat-barrier coating ceramic layer of anti-CMAS corrosion of the present invention, packet
The following steps are included：
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Second step：The preparation of air plasma spraying powder；
The grain size that the present invention prepares powder used in the second ceramic layer is 30~50 μm.
Third walks：Air plasma spraying method prepares the second ceramic layer；
Technological parameter is：Spray power is 20~40KW, and spray distance is 100~150mm, and powder feed rate is 8~12g/
The movement speed of min, lateral plasma gun are 500 μm/s, and Ar throughputs are 80slpm, H2Throughput is 30slpm, the second pottery
The deposition thickness of enamel coating is 100~250 μm, further preferably 120~170 μm.
The advantage of the invention is that：
1, the analysis according to XRD, SEM and EDS to prepared ceramic layer performance adjusts spraying parameter and materials chemistry
Ingredient ratio obtains the single-phase LaPO for meeting stoichiometric ratio4Ceramic layer.
2, preparation method simple possible, it is easily controllable.
3, the heat-barrier coating ceramic layer for the anti-CMAS corrosion that prepared by the present invention is poor to the wetability for melting CMAS, 1250 DEG C
After being heat-treated 30h, in CMAS layer and one layer of mutual reactance layer of the second ceramic layer interface formation, effectively prevent that CMAS's is further
It penetrates into, YSZ ceramic layers maintain original phase stability, and the second ceramic layer has good anti-CMAS corrosive natures.
Description of the drawings
Fig. 1 is the shape appearance figure that air plasma spraying method prepares the optimization pelletizing that the second ceramic layer uses；
Fig. 2 is that air plasma spraying method prepares LaPO4The XRD material phase analysis figures of ceramic layer；
Fig. 3 is LaPO prepared by air plasma spraying method4The Cross Section Morphology figure of ceramic layer；
Fig. 4 is LaPO prepared by air plasma spraying method4Surface ceramii layer coating CMAS powder is heat-treated 30h at 1250 DEG C
Cross Section Morphology figure afterwards；
Fig. 5 is LaPO prepared by air plasma spraying method4Ceramic layer CMAS after different time is heat-treated penetrates into deep
The curve graph of degree.
Specific implementation mode：
Below in conjunction with drawings and examples, the present invention is described in further detail.
The present invention provides a kind of air plasma spraying preparation method of the heat-barrier coating ceramic layer of anti-CMAS corrosion, described
Preparation method include the following steps：
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts into the thin slice of 15mm × 20mm × 2mm, by the matrix of well cutting
Sample uses the SiC silicon carbide papers of 400#, 600#, 800# to polish successively, and sandblasting pretreatment is to increase Substrate Surface Roughness (Ra ＜
2)；The matrix sample of sandblasting pretreatment is cleaned into 10min with acetone and EtOH Sonicate ripple successively, is dried, it is spare.
Using Metco 7M plasma spraying equipments sandblasting pretreatment Al2O3YSZ ceramic layers are prepared on matrix sample,
Spray power is 30KW, spray distance 150mm, powder feed rate 10g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the deposition thickness of YSZ ceramic layers is 100 μm.
Second step：The preparation of air plasma spraying powder；
The present invention is prepared powder used in the second ceramic layer and is prepared using drying process with atomizing, and the grain size of powder is 30~50 μ
m。
Third walks：Air plasma spraying method prepares the second ceramic layer；
Second ceramic layer, spray power 20 are deposited in YSZ surface ceramii layers using Metco 7M plasma spraying equipments
~40KW, spray distance are 100~150mm, and powder feed rate is 8~12g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the second ceramic layer deposition thickness is 100~250 μm.
CMAS powder is studied into its anti-CMAS corrosive nature coated in the second surface ceramii layer, second ceramic layer is to melting
The wetability of CMAS is poor, and after 1250 DEG C of heat treatment 30h, one layer of mutual reactance is formed in CMAS layers and the second ceramic layer interface
Layer effectively prevents penetrating further into for CMAS, YSZ ceramic layers to maintain original phase stability, and the second ceramic layer has good
Good anti-CMAS corrosive natures.
Embodiment 1：Select LaP3O9Powder prepares the second ceramic layer；
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts into the thin slice of 15mm × 20mm × 2mm, by the matrix of well cutting
Sample uses the SiC silicon carbide papers of 400#, 600#, 800# to polish successively, and sandblasting pretreatment is to increase Substrate Surface Roughness (Ra ＜
2)；The matrix sample of sandblasting pretreatment is cleaned into 10min with acetone and EtOH Sonicate ripple successively, is dried, it is spare.
Using Metco 7M plasma spraying equipments sandblasting pretreatment Al2O3YSZ ceramic layers are prepared on matrix sample,
Spray power is 30KW, spray distance 150mm, powder feed rate 10g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the deposition thickness of YSZ ceramic layers is 100 μm.
Second step：The preparation of air plasma spraying powder；
Using LaP3O9Powder prepares the second ceramic layer, LaP3O9Powder is prepared using drying process with atomizing, preparation
LaP3O9Morphology microstructure is as shown in Figure 1, LaP3O9The grain size of powder is between 30~50 μm.
Third walks：Air plasma spraying method prepares the second ceramic layer；
LaP is sprayed in YSZ surface ceramii layers using Metco 7M plasma spraying equipments3O9Powder is ceramic to deposit second
Layer, spray power 30KW, spray distance 100mm, powder feed rate 10g/min, the movement speed of lateral plasma gun are
500 μm/s, Ar throughputs are 80slpm, H2Throughput is 30slpm, and the deposition thickness of the second ceramic layer is 150 μm.
The ingredient that the second ceramic layer is made is analyzed using EDS, energy spectrum composition analysis the results are shown in Table 1, it can be seen that
The atomic ratio that La and P in the second ceramic layer is made is 1:1.XRD analysis collection of illustrative plates as shown in Fig. 2, XRD material phase analysis the result shows that
Two ceramic layers are the LaPO of the solitary stone structure of monoclinic phase4, the second ceramic layer is LaPO in the present embodiment4Ceramic layer.It is made
LaPO4The Cross Section Morphology of ceramic layer is fig. 3, it is shown that LaPO4Ceramic layer structure is fine and close, and hole is less, with YSZ ceramics
Layer combines preferable.
CMAS powder is respectively coated on LaPO4The granularity of ceramic layer and YSZ surface ceramii layers, the CMAS powder is 60 μm,
The coating density of CMAS powder is 30mg/cm2；Two groups of samples are used after 1250 DEG C are heat-treated 5h, 10h, 30h and 90h respectively
SEM observation analysis, surface coat the LaPO of CMAS powder4Ceramic layer is heat-treated Cross Section Morphology figure such as Fig. 4 after 30h at 1250 DEG C,
Ca, Si element be can be seen that from LaPO4Surface ceramii layer is to LaPO4It penetrates into inside ceramic layer, Ca, Si and La react generation
The formation of silicate oxyapatite phase, a large amount of silicate oxyapatite phases causes in LaPO4Ceramic layer and the bed boundarys CMAS
Place forms one layer of mutual reactance layer, effectively prevents Ca, Si penetrating further into YSZ ceramic layers.At 1250 DEG C, mutual reactance layer
The relationship of thickness and heat treatment time as shown in figure 5, heat treatment 30h when mutual reactance layer thickness reach 35 μm, hereafter with heat at
The extension mutual reactance layer thickness of reason time no longer obviously increases, and illustrates in the case where CMAS is acted on, 1250 DEG C of heat treatment times reach
After to 30h there is certain thickness mutual reactance layer to have prevented penetrating further into for CMAS, YSZ ceramic layers maintain original
Some phase stabilities select LaP3O9Single-phase LaPO prepared by powder4Ceramic layer has good anti-CMAS erosion performances.
Control group 1：Select LaPO4Powder prepares the second ceramic layer；
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts into the thin slice of 15mm × 20mm × 2mm, by the matrix of well cutting
Sample uses the SiC silicon carbide papers of 400#, 600#, 800# to polish successively, and sandblasting pretreatment is to increase Substrate Surface Roughness (Ra ＜
2)；The matrix sample of sandblasting pretreatment is cleaned into 10min with acetone and EtOH Sonicate ripple successively, is dried, it is spare.
Using Metco 7M plasma spraying equipments sandblasting pretreatment Al2O3YSZ ceramic layers are prepared on matrix sample,
Spray power is 30KW, spray distance 150mm, powder feed rate 10g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the deposition thickness of YSZ ceramic layers is 100 μm.
Second step：The preparation of air plasma spraying powder；
LaPO is prepared using drying process with atomizing4Powder, LaPO4The grain size of powder is 40~50 μm.
Third walks：Air plasma spraying method prepares the second ceramic layer；
LaPO is sprayed in YSZ surface ceramii layers using Metco 7M plasma spraying equipments4Powder is ceramic to deposit second
Layer, spray power 30KW, spray distance 100mm, powder feed rate 10g/min, the movement speed of lateral plasma gun are
500 μm/s, Ar throughputs are 80slpm, H2Throughput is 30slpm, and the deposition thickness of the second ceramic layer is 150 μm.
Second ceramic layer structure is fine and close, but the second ceramic layer component distributing is uneven, there are melting zone and non-melting zone, by
In LaPO4Different with the vapour pressure of phosphoric acid, the second ceramic layer melting zone existence component segregation, EDS analysis results show melting zone
The atomic ratio of La and P is 3:1, non-melting zone La and P atomic ratios are 1:1.
Control group 2：Select LaP5O14Powder prepares the second ceramic layer；
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts into the thin slice of 15mm × 20mm × 2mm, by the matrix of well cutting
Sample uses the SiC silicon carbide papers of 400#, 600#, 800# to polish successively, and sandblasting pretreatment is to increase Substrate Surface Roughness (Ra ＜
2)；The matrix sample of sandblasting pretreatment is cleaned into 10min with acetone and EtOH Sonicate ripple successively, is dried, it is spare.
Using Metco 7M plasma spraying equipments sandblasting pretreatment Al2O3YSZ ceramic layers are prepared on matrix sample,
Spray power is 30KW, spray distance 150mm, powder feed rate 10g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the deposition thickness of YSZ ceramic layers is 100 μm.
Second step：The preparation of air plasma spraying powder；
LaP is prepared using drying process with atomizing5O14Powder, LaP5O14The grain size of powder is 40~50 μm.
Third walks：Air plasma spraying method prepares the second ceramic layer；
LaP is sprayed in YSZ surface ceramii layers using Metco 7M plasma spraying equipments5O14Powder is ceramic to deposit second
Layer, spray power 30KW, spray distance 100mm, powder feed rate 10g/min, the movement speed of lateral plasma gun are
500 μm/s, Ar throughputs are 80slpm, H2Throughput is 30slpm, and the deposition thickness of the second ceramic layer is 150 μm.
The ingredient of the second ceramic layer is analyzed using EDS, analysis result shows that the atomic ratio of La and P is 1:1.5, deviate
LaPO4Stoichiometric ratio；The surface topography that the second ceramic layer is made is analyzed using SEM, the second surface ceramii layer hole
Gap is more, and structure is not fine and close, and it is poor to be combined with YSZ ceramic layers.
1 LaPO of table4The power spectrum ingredient of ceramic layer
Embodiment 2：Select LaP3O9Powder prepares the second ceramic layer；
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts into the thin slice of 15mm × 20mm × 2mm, by the matrix of well cutting
Sample uses the SiC silicon carbide papers of 400#, 600#, 800# to polish successively, and sandblasting pretreatment is to increase Substrate Surface Roughness (Ra ＜
2)；The matrix sample of sandblasting pretreatment is cleaned into 10min with acetone and EtOH Sonicate ripple successively, is dried, it is spare.
Using Metco 7M plasma spraying equipments sandblasting pretreatment Al2O3YSZ ceramic layers are prepared on matrix sample,
Spray power is 30KW, spray distance 150mm, powder feed rate 10g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the deposition thickness of YSZ ceramic layers is 100 μm.
Second step：The preparation of air plasma spraying powder；
LaP is prepared using drying process with atomizing3O9Powder, LaP3O9The grain size of powder is 30~50 μm.
Third walks：Air plasma spraying method prepares the second ceramic layer；
LaP is sprayed in YSZ surface ceramii layers using Metco 7M plasma spraying equipments3O9Powder is ceramic to deposit second
Layer, spray power 35KW, spray distance 100mm, powder feed rate 10g/min, the movement speed of lateral plasma gun are
500 μm/s, Ar throughputs are 80slpm, H2Throughput is 30slpm, and the deposition thickness of the second ceramic layer is 170 μm.
Constituent analysis is carried out using EDS pairs of the second ceramic layer, analysis result shows the atomic ratio of La and P in the second ceramic layer
It is 5:3, XRD material phase analysis are the result shows that the second ceramic layer obtained is not the LaPO of the solitary stone structure of single monoclinic phase4,
Other object phases are also equipped with, the second ceramic layer prepared in the present embodiment is non-single-phase LaPO4Ceramic layer；Second ceramic layer structure causes
Close, hole is less.
CMAS powder is coated in the second surface ceramii layer prepared, the granularity of the CMAS powder is 60 μm, the painting of CMAS powder
It is 30mg/cm to cover density2；Sample is after 1250 DEG C are heat-treated 5h, 10h, 30h and 90h respectively, with SEM observation analysis samples
Cross Section Morphology, Ca, Si element from the second surface ceramii layer to the second ceramic layer inside penetrate into, Ca, Si and La react generation
Silicate oxyapatite phase, the formation of a large amount of silicate oxyapatite phases cause in the second ceramic layer and the bed boundarys CMAS
Place forms one layer of mutual reactance layer, effectively prevents Ca, Si penetrating further into YSZ ceramic layers.Study 1250 DEG C of mutual reactance layers
Thickness and heat treatment time relationship, be heat-treated 30h when mutual reactance layer thickness reach 25 μm, hereafter with heat treatment time
Extend mutual reactance layer thickness no longer to obviously increase, illustrate in the case where CMAS is acted on, 1250 DEG C of heat treatment times have after reaching 30h
There is certain thickness mutual reactance layer to prevent penetrating further into for CMAS, YSZ ceramic layers maintain original mutually steady
It is qualitative, select LaP3O9Second ceramic layer prepared by powder has good anti-CMAS erosion performances.
Control group 1：Select LaPO4Powder prepares the second ceramic layer；
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts into the thin slice of 15mm × 20mm × 2mm, by the matrix of well cutting
Sample uses the SiC silicon carbide papers of 400#, 600#, 800# to polish successively, and sandblasting pretreatment is to increase Substrate Surface Roughness (Ra ＜
2)；The matrix sample of sandblasting pretreatment is cleaned into 10min with acetone and EtOH Sonicate ripple successively, is dried, it is spare.
Using Metco 7M plasma spraying equipments sandblasting pretreatment Al2O3YSZ ceramic layers are prepared on matrix sample,
Spray power is 30KW, spray distance 150mm, powder feed rate 10g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the deposition thickness of YSZ ceramic layers is 100 μm.
Second step：The preparation of air plasma spraying powder；
LaPO is prepared using drying process with atomizing4Powder, LaPO4The grain size of powder is 40~50 μm.
Third walks：Air plasma spraying method prepares the second ceramic layer；
LaPO is sprayed in YSZ surface ceramii layers using Metco 7M plasma spraying equipments4Powder is ceramic to deposit second
Layer, spray power 35KW, spray distance 100mm, powder feed rate 10g/min, the movement speed of lateral plasma gun are
500 μm/s, Ar throughputs are 80slpm, H2Throughput is 30slpm, and the deposition thickness of the second ceramic layer is 170 μm.
Second ceramic layer structure is fine and close, but component distributing is uneven, and there are melting zones and non-melting zone, due to LaPO4With
The vapour pressure of phosphoric acid is different, and the melting zone existence component segregation of the second ceramic layer, EDS analysis results show melting zone La and P
Atomic ratio is 3:1, non-melting zone La and P atomic ratios are 1:1.
Control group 2：Select LaP5O14Powder prepares the second ceramic layer；
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts into the thin slice of 15mm × 20mm × 2mm, by the matrix of well cutting
Sample uses the SiC silicon carbide papers of 400#, 600#, 800# to polish successively, and sandblasting pretreatment is to increase Substrate Surface Roughness (Ra ＜
2)；The matrix sample of sandblasting pretreatment is cleaned into 10min with acetone and EtOH Sonicate ripple successively, is dried, it is spare.
Using Metco 7M plasma spraying equipments sandblasting pretreatment Al2O3YSZ ceramic layers are prepared on matrix sample,
Spray power is 30KW, spray distance 150mm, powder feed rate 10g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the deposition thickness of YSZ ceramic layers is 100 μm.
Second step：The preparation of air plasma spraying powder；
LaP is prepared using drying process with atomizing5O14Powder, LaP5O14The grain size of powder is 40~50 μm.
Third walks：Air plasma spraying method prepares the second ceramic layer；
LaP is sprayed in YSZ surface ceramii layers using Metco 7M plasma spraying equipments5O14Powder is ceramic to deposit second
Layer, spray power 35KW, spray distance 100mm, powder feed rate 10g/min, the movement speed of lateral plasma gun are
500 μm/s, Ar throughputs are 80slpm, H2Throughput is 30slpm, and the deposition thickness of the second ceramic layer is 170 μm.
The ingredient of the second ceramic layer is analyzed using EDS, analysis result shows that the atomic ratio of La and P is 1:1.5, deviate
LaPO4Stoichiometric ratio；The surface topography that the second ceramic layer is made is analyzed using SEM, the second surface ceramii layer hole
Gap is more, and structure is not fine and close, and it is poor to be combined with YSZ ceramic layers.
Embodiment 3：Select LaP3O9Powder prepares the second ceramic layer；
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts into the thin slice of 15mm × 20mm × 2mm, by the matrix of well cutting
Sample uses the SiC silicon carbide papers of 400#, 600#, 800# to polish successively, and sandblasting pretreatment is to increase Substrate Surface Roughness (Ra ＜
2)；The matrix sample of sandblasting pretreatment is cleaned into 10min with acetone and EtOH Sonicate ripple successively, is dried, it is spare.
Using Metco 7M plasma spraying equipments sandblasting pretreatment Al2O3YSZ ceramic layers are prepared on matrix sample,
Spray power is 30KW, spray distance 150mm, powder feed rate 10g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the deposition thickness of YSZ ceramic layers is 100 μm.
Second step：The preparation of air plasma spraying powder；
LaP is prepared using drying process with atomizing3O9Powder, LaP3O9The grain size of powder is 30~50 μm.
Third walks：Air plasma spraying method prepares the second ceramic layer；
LaP is sprayed in YSZ surface ceramii layers using Metco 7M plasma spraying equipments3O9Powder is ceramic to deposit second
Layer, spray power 35KW, spray distance 120mm, powder feed rate 10g/min, the movement speed of lateral plasma gun are
500 μm/s, Ar throughputs are 80slpm, H2Throughput is 30slpm, and the deposition thickness of the second ceramic layer is 120 μm.
It is analyzed using the ingredient of EDS pairs of the second ceramic layer, analysis result shows the atom of La and P in the second ceramic layer
Than being 4:3, XRD material phase analysis show that the second ceramic layer is not the LaPO of the solitary stone structure of single monoclinic phase4, obtained
Two ceramic layer structures are fine and close, and hole is less, is well combined with YSZ ceramic layers.
CMAS powder is coated in the second surface ceramii layer prepared, the granularity of the CMAS powder is 60 μm, the painting of CMAS powder
It is 30mg/cm to cover density2；Sample is after 1250 DEG C are heat-treated 5h, 10h, 30h and 90h respectively, with SEM observation analysis samples
Cross Section Morphology, Ca, Si element from the second surface ceramii layer to the second ceramic layer inside penetrate into, Ca, Si and La react generation
The formation of silicate oxyapatite phase, a large amount of silicate oxyapatite phases causes at the second ceramic layer and the bed boundarys CMAS
One layer of mutual reactance layer is formed, Ca, Si penetrating further into YSZ ceramic layers are effectively prevented.1250 DEG C of mutual reactance layers of research
The relationship of thickness and heat treatment time, mutual reactance layer thickness reaches 30 μm when being heat-treated 30h, hereafter prolonging with heat treatment time
Long mutual reactance layer thickness no longer obviously increases, and illustrates in the case where CMAS is acted on, 1250 DEG C of heat treatment times have after reaching 30h
Certain thickness mutual reactance layer has prevented penetrating further into for CMAS, and YSZ ceramic layers maintain original phase and stablize
Property, select LaP3O9Second ceramic layer prepared by powder has good anti-CMAS erosion performances.
Control group 1：Select LaPO4Powder prepares the second ceramic layer；
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts into the thin slice of 15mm × 20mm × 2mm, by the matrix of well cutting
Sample uses the SiC silicon carbide papers of 400#, 600#, 800# to polish successively, and sandblasting pretreatment is to increase Substrate Surface Roughness (Ra ＜
2)；The matrix sample of sandblasting pretreatment is cleaned into 10min with acetone and EtOH Sonicate ripple successively, is dried, it is spare.
Using Metco 7M plasma spraying equipments sandblasting pretreatment Al2O3YSZ ceramic layers are prepared on matrix sample,
Spray power is 30KW, spray distance 150mm, powder feed rate 10g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the deposition thickness of YSZ ceramic layers is 100 μm.
Second step：The preparation of air plasma spraying powder；
LaPO is prepared using drying process with atomizing4Powder, LaPO4The grain size of powder is 40~50 μm.
Third walks：Air plasma spraying method prepares LaPO4Ceramic layer；
LaPO is sprayed in YSZ surface ceramii layers using Metco 7M plasma spraying equipments4Powder is ceramic to deposit second
Layer, spray power 35KW, spray distance 120mm, powder feed rate 10g/min, the movement speed of lateral plasma gun are
500 μm/s, Ar throughputs are 80slpm, H2Throughput is 30slpm, and the deposition thickness of the second ceramic layer is 120 μm.
Second ceramic layer structure is fine and close, but component distributing is uneven, and there are melting zones and non-melting zone, due to LaPO4With
The vapour pressure of phosphoric acid is different, and the second ceramic layer melting zone existence component segregation, EDS analysis results show the original of melting zone La and P
Son is than being 3:1, non-melting zone La and P atomic ratios are 1:1.
Control group 2：Select LaP5O14Powder prepares the second ceramic layer；
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts into the thin slice of 15mm × 20mm × 2mm, by the matrix of well cutting
Sample uses the SiC silicon carbide papers of 400#, 600#, 800# to polish successively, and sandblasting pretreatment is to increase Substrate Surface Roughness (Ra ＜
2)；The matrix sample of sandblasting pretreatment is cleaned into 10min with acetone and EtOH Sonicate ripple successively, is dried, it is spare.
Using Metco 7M plasma spraying equipments sandblasting pretreatment Al2O3YSZ ceramic layers are prepared on matrix sample,
Spray power is 30KW, spray distance 150mm, powder feed rate 10g/min, and the movement speed of lateral plasma gun is 500 μ
M/s, Ar throughput are 80slpm, H2Throughput is 30slpm, and the deposition thickness of YSZ ceramic layers is 100 μm.
Second step：The preparation of air plasma spraying powder；
LaP is prepared using drying process with atomizing5O14Powder, LaP5O14The grain size of powder is 40~50 μm.
Third walks：Air plasma spraying method prepares the second ceramic layer；
LaP is sprayed in YSZ surface ceramii layers using Metco 7M plasma spraying equipments5O14Powder is ceramic to deposit second
Layer, spray power 35KW, spray distance 120mm, powder feed rate 10g/min, the movement speed of lateral plasma gun are
500 μm/s, Ar throughputs are 80slpm, H2Throughput is 30slpm, and the deposition thickness of the second ceramic layer is 120 μm.
The ingredient of the second ceramic layer is analyzed using EDS, analysis result shows that the atomic ratio of La and P is 1:1.5, deviate
LaPO4Stoichiometric ratio；The surface topography that the second ceramic layer is made is analyzed using SEM, the second surface ceramii layer hole
Gap is more, and structure is not fine and close, and it is poor to be combined with YSZ ceramic layers.
Claims (3)
1. a kind of air plasma spraying preparation method of the heat-barrier coating ceramic layer of anti-CMAS corrosion, it is characterised in that：It is described
Preparation method includes the following steps,
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts flakiness, and the matrix sample polishing of well cutting, sandblasting, ultrasonic wave is clear
The pretreatment washed and dried；Al after the pre-treatment2O3The first ceramic layer is prepared on matrix sample --- YSZ ceramic layers, YSZ potteries
The deposition thickness of enamel coating is 100 μm；
Second step：The preparation of air plasma spraying powder；The air plasma spraying is LaP with powder3O9Powder,
The grain size of powder is 30~50 μm；
Third walks：Air plasma spraying method prepares the second ceramic layer；
The second ceramic layer is deposited in YSZ surface ceramii layers, technological parameter is：Spray power 30KW, spray distance 100mm, send
Powder speed is 10g/min, and the speed of lateral plasma gun is 500 μm/s, and Ar throughputs are 80slpm, H2Throughput is
The deposition thickness of 30slpm, the second ceramic layer are 150 μm；
The atomic ratio of La and P is 1 in second ceramic layer:1, XRD material phase analysis is the result shows that the second ceramic layer is that monoclinic phase is solitary
The LaPO of stone structure4。
2. a kind of application of the heat-barrier coating ceramic layer of anti-CMAS corrosion, it is characterised in that：The thermal boundary of the anti-CMAS corrosion applies
Layer ceramic layer is prepared using preparation method in claim 1；The heat-barrier coating ceramic layer surface coats CMAS,
After 1250 DEG C of heat treatment, mutual reactance layer is formed in the second ceramic layer and the interfaces CMAS, prevents penetrating further into for CMAS,
YSZ ceramic layers maintain original phase stability.
3. a kind of thermal barrier coating of anti-CMAS corrosion, it is characterised in that：The thermal barrier coating includes being sequentially prepared on matrix
YSZ ceramic layers and the second ceramic layer, the thickness of YSZ ceramic layers is 200 μm, and the thickness of the second ceramic layer is 150 μm；
The coating is prepared as follows to obtain：
The first step：Substrate pretreated, and the first ceramic layer is prepared on matrix after the pre-treatment --- YSZ ceramic layers；
Using the method for wire cutting by Al2O3Matrix cuts flakiness, and the matrix sample polishing of well cutting, sandblasting, ultrasonic wave is clear
The pretreatment washed and dried；Al after the pre-treatment2O3The first ceramic layer is prepared on matrix sample --- YSZ ceramic layers, YSZ potteries
The deposition thickness of enamel coating is 100 μm；
Second step：The preparation of air plasma spraying powder；The air plasma spraying is LaP with powder3O9Powder,
The grain size of powder is 30~50 μm；
Third walks：Air plasma spraying method prepares the second ceramic layer；
The second ceramic layer is deposited in YSZ surface ceramii layers, technological parameter is：Spray power 30KW, spray distance 100mm, send
Powder speed is 10g/min, and the speed of lateral plasma gun is 500 μm/s, and Ar throughputs are 80slpm, H2Throughput is
The deposition thickness of 30slpm, the second ceramic layer are 150 μm；The atomic ratio for obtaining meeting La and P in the second ceramic layer is 1:1 list
The LaPO of the solitary stone structure of monoclinic phase4Ceramic layer.
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| FR3067391B1 (en) | 2017-06-12 | 2020-12-04 | Safran | REINFORCED ANTI-CMAS COATING |
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| CN110284097B (en) * | 2019-08-13 | 2021-04-09 | 广东省新材料研究所 | Environmental barrier coating and coating method and application thereof |
| CN112941451B (en) * | 2021-01-25 | 2022-08-05 | 武汉理工大学 | Method for improving stability of thermal barrier coating in natural environment |
| CN114671686B (en) * | 2022-04-21 | 2023-09-22 | 昆明理工大学 | Preparation method of ceramic material capable of fast reacting with low-melting-point oxide and resisting permeation |
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