The specific embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
The present invention is a kind of high temperature resistance (1000~1250 ℃) oxidation Al
2O
3/ Al-Si-Cr composite coating, described Al
2O
3/ Al-Si-Cr composite coating is by Al
2O
3Coating and Al-Si-Cr mixed layer form, Al
2O
3Coating is between Al-Si-Cr mixed layer and Nb-24Ti-16Si-6Al-6Cr-2Hf matrix.Described Al
2O
3Coating layer thickness is 50~200 μ m.Described Al-Si-Cr mixed layer thickness is 50~200 μ m, and this coating is by Cr (Si, Al)
2, Al, Si three phase compositions, Al-Si-Cr mixed layer surface is formed with Al when 1000~1250 ℃ of oxidation 100h of high temperature
2O
3And SiO
2Mixed oxide layer.
The present invention is a kind of employing low pressure 30~40 * 10
3The pa plasma spraying prepares Al
2O
3The method of/Al-Si-Cr composite coating, this coating production has the following step:
The first step: the pre-treatment of matrix
With Nb-24Ti-16Si-6Al-6Cr-2Hf matrix adopting 150#, 360#, the polishing of 500# silicon carbide paper, and it is back stand-by to adopt sand-blasting machine to carry out the surface sand-blasting processing, matrix surface roughness RZ=60 after the sandblast~80 μ m;
Second step: preparation Al-Si-Cr coating material
(A) take by weighing the Al powder of 30~35wt%, the Cr powder of 30~33wt%, the Si powder of 32~40wt%, and the content sum of above-mentioned each composition is 100%, mixes after grind that to make granularity behind 30~150min be 250~350 purposes, first mixed-powders;
(B) will mix with binding agent through first mixed-powder that (A) step makes after to make granularity after grinding 250~400min be 250~350 purposes, second mixed-powders;
The consumption of first mixed-powder and binding agent is a binding agent of putting into 1000~1500ml in first mixed-powder of 1000g;
Described binding agent is stirred in 80~100 ℃ by gum arabic and deionized water and makes, and the consumption of gum arabic and deionized water is to add 0.5~5g gum arabic in every 100ml deionized water;
(C) will make granularity through second mixed-powder that (B) step makes after the atomization drying granulation is 200~250 purpose coating materials;
Atomization drying adopts centrifugal atomizing method, it (is coating material that the shearing force that second mixed-powder injects atomizer and is atomized device immediately through constant flow pump is dispersed into a lot of fine drop, its particle diameter is 40~80 μ m), wherein the atomizer rotating speed is 8000~20000r/min, the atomizer inlet temperature is 220~230 ℃, and the atomizer outlet temperature is 130~150 ℃;
The 3rd step: preparation Al
2O
3Coating material
Choose the Al that granularity is 200~250 purpose purity 99.9%
2O
3Spheroidal powder material;
The 4th step: low-voltage plasma spraying system coating
(A) matrix after the first step is processed is installed on the anchor clamps of low-voltage plasma spraying equipment, and will be through the Al of the 3rd step preparation
2O
3Coating material is put into feed appliance, regulates spraying parameter Al processed
2O
3Coating;
Plasma spraying parameter: jar internal pressure 30~40 * 10
3Pa, the primary air amount is 60~100L/h, and inferior throughput is 25~30L/h, and arc current is 560~600A, and arc voltage is 50~60V, the powder sending quantity of powder feeder is 24~25g/min;
(B) second step preparation Al-Si-Cr coating material is put into feed appliance, regulate spraying parameter system Al-Si-Cr coating;
Plasma spraying parameter: jar internal pressure 30~40 * 10
3Pa, the primary air amount is 60~100L/h, and inferior throughput is 25~30L/h, and electric current is 560~600A, and voltage is 50~60V, the powder sending quantity of powder feeder is 20~22g/min.
Al with the said method preparation
2O
3/ Al-Si-Cr composite coating shows that through XRD, sem analysis the Al-Si-Cr mixed coating is by Cr (Si, Al)
2, Al, Si three phase compositions, this coating is formed with Al with interior on Al-Si-Cr mixed layer surface at 1000~1250 ℃ of oxidation 100h of high temperature
2O
3And SiO
2Mixed oxide layer.
Embodiment 1:
The first step: the pre-treatment of matrix
With Nb-24Ti-16Si-6Al-6Cr-2Hf matrix cut growth 13mm, wide 8mm, the rectangle sample of high 3mm, and after adopting 150#, 360#, the polishing of 500# silicon carbide paper, it is stand-by that the employing sand-blasting machine carries out surface sand-blasting processing back, matrix surface roughness RZ=60 after the sandblast~80 μ m;
Second step: preparation coating material
(A) the Si powder that takes by weighing Cr powder, the 34.6wt% of Al powder, the 32.1wt% of 33.3wt% mixes after grind that to make granularity behind the 100min be 250~350 purposes, first mixed-powders;
(B) will mix with binding agent through first mixed-powder that (A) step makes after to make granularity after grinding 300min be 250~350 purposes, second mixed-powders;
The consumption of first mixed-powder and binding agent is a binding agent of putting into 1000ml in first mixed-powder of 1000g;
Described binding agent is stirred in 100 ℃ by gum arabic and deionized water and makes, and the consumption of gum arabic and deionized water is to add the 1g gum arabic in every 100ml deionized water;
(C) will make granularity through second mixed-powder that (B) step makes after the atomization drying granulation is 200~250 purpose coating materials;
Atomization drying adopts centrifugal atomizing method, second mixed-powder is dispersed into a lot of fine drop (particle diameter is 60~80 μ m) through the shearing force that constant flow pump injection atomizer also is atomized device immediately, wherein the atomizer rotating speed is 15000r/min, 225 ℃ of atomizer inlet temperatures, atomizer outlet temperature are 140 ℃.
The 3rd step: preparation Al
2O
3Coating material
Choose the Al that granularity is 200~250 purpose purity 99.9%
2O
3Spheroidal powder material;
The 4th step: low-voltage plasma spraying system coating
(A) matrix after the first step is processed is installed on the anchor clamps of low-voltage plasma spraying equipment, and will be through the Al of the 3rd step preparation
2O
3Coating material is put into feed appliance, regulates spraying parameter Al processed
2O
3Coating;
Plasma spraying parameter: jar internal pressure 30 * 10
3Pa, the primary air amount is 60L/h, and inferior throughput is 25L/h, and electric current is 580A, and voltage is 55V, the powder sending quantity of powder feeder is 24g/min;
(B) second step preparation Al-Si-Cr coating material is put into feed appliance, regulate spraying parameter system Al-Si-Cr coating;
Plasma spraying parameter: jar internal pressure 30 * 10
3Pa, the primary air amount is 60L/h, and inferior throughput is 25L/h, and electric current is 580A, and voltage is 55V, the powder sending quantity of powder feeder is 21g/min.
With the above-mentioned Al that makes
2O
3/ Al-Si-Cr composite coating shows through sem analysis, the Al of preparation
2O
3/ Al-Si-Cr composite coating mainly is made up of two-layer: outer is the Al-Si-Cr mixed layer, and this mixed layer is by Cr (Si, Al)
2, Al, Si three phase compositions; Internal layer is the Al between coating and the matrix
2O
3Coating, its section structure signal as shown in Figure 1.
In air atmosphere, during through 1250 ℃ of isothermal oxidation 100h, the weightening finish of matrix surface unit are is 213mg/cm with the Nb-24Ti-16Si-6Al-6Cr-2Hf matrix
2
To make Al
2O
3The matrix of/Al-Si-Cr composite coating is in air atmosphere, and during through 1250 ℃ of isothermal oxidation 100h, the weightening finish of coating surface unit are is 9.8mg/cm
2Find (section structure is illustrated as shown in Figure 2) by the sem analysis to the oxidised samples section, coating mainly forms by three layers after the oxidation: skin is Al
2O
3And SiO
2Mixed oxide layer; The intermediate layer is the Al-Si-Cr mixed layer; Internal layer is Al
2O
3Coating (100 μ m are arranged approximately).Coating surface after the oxidation shows that through XRD, sem analysis coating surface has formed continuous, fine and close Al
2O
3And SiO
2Mixed oxide layer, thus the diffusion of oxygen to matrix successfully stoped.
By not comparing with preparing coating of material preparing cated matrix, its unit are weightening finish has reduced about 200mg/m
2, prove that the cated matrix of preparation has good high-temperature oxidation resistant effect.
Embodiment 2:
The first step: the pre-treatment of matrix
With Nb-24Ti-16Si-6Al-6Cr-2Hf matrix cut growth 13mm, wide 8mm, the rectangle sample of high 3mm, and after adopting 150#, 360#, the polishing of 500# silicon carbide paper, it is stand-by that the employing sand-blasting machine carries out surface sand-blasting processing back, matrix surface roughness RZ=60 after the sandblast~80 μ m;
Second step: preparation coating material
(A) the Si powder that takes by weighing Cr powder, the 40wt% of Al powder, the 30wt% of 30wt% mixes after grind that to make granularity behind the 150min be 250~350 purposes, first mixed-powders;
(B) will mix with binding agent through first mixed-powder that (A) step makes after to make granularity after grinding 400min be 250~350 purposes, second mixed-powders;
The consumption of first mixed-powder and binding agent is a binding agent of putting into 1500ml in first mixed-powder of 1000g;
Described binding agent is stirred in 80 ℃ by gum arabic and deionized water and makes, and the consumption of gum arabic and deionized water is to add the 5g gum arabic in every 100ml deionized water;
(C) will make granularity through second mixed-powder that (B) step makes after the atomization drying granulation is 200~250 purpose coating materials;
Atomization drying adopts centrifugal atomizing method, second mixed-powder is dispersed into a lot of fine drop (particle diameter is 40~70 μ m) through the shearing force that constant flow pump injection atomizer also is atomized device immediately, wherein the atomizer rotating speed is 20000r/min, the atomizer inlet temperature is 230 ℃, and the atomizer outlet temperature is 150 ℃.
The 3rd step: preparation Al
2O
3Coating material
Choose the Al that granularity is 200~250 purpose purity 99.9%
2O
3Spheroidal powder material;
The 4th step: low-voltage plasma spraying system coating
(A) matrix after the first step is processed is installed on the anchor clamps of low-voltage plasma spraying equipment, and will be through the Al of the 3rd step preparation
2O
3Coating material put into feed appliance, regulate spraying parameter Al processed
2O
3Coating;
Plasma spraying parameter: jar internal pressure 40 * 10
3Pa, the primary air amount is 100L/h, and inferior throughput is 30L/h, and electric current is 600A, and voltage is 60V, the powder sending quantity of powder feeder is 25g/min;
(B) second step preparation Al-Si-Cr coating material is put into feed appliance, regulate spraying parameter system Al-Si-Cr mixed coating;
Plasma spraying parameter: jar internal pressure 40 * 10
3Pa, the primary air amount is 100L/h, and inferior throughput is 30L/h, and electric current is 600A, and voltage is 60V, the powder sending quantity of powder feeder is 22g/min.
With the above-mentioned Al that makes
2O
3/ Al-Si-Cr composite coating shows that through sem analysis the coating of preparation mainly is made up of two-layer: outer is the Al-Si-Cr mixed layer, Cr (Si, Al) in this mixed layer
2, Al, Si three phase compositions; Internal layer is the Al between coating and the matrix
2O
3Coating.
In air atmosphere, during through 1000 ℃ of isothermal oxidation 100h, the weightening finish of matrix surface unit are is 44.6mg/cm with the Nb-24Ti-16Si-6Al-6Cr-2Hf matrix
2
In air atmosphere, during through 1000 ℃ of isothermal oxidation 100h, the weightening finish of coating surface unit are is 4.2mg/cm with the matrix that makes the Al-Si-Cr coating
2Find that by the sem analysis to the oxidised samples section coating mainly forms by three layers after the oxidation: skin is Al
2O
3And SiO
2Mixed oxide layer; The intermediate layer is the Al-Si-Cr mixed layer; Internal layer is Al
2O
3Layer (200 μ m are arranged approximately).Coating surface after the oxidation shows that through XRD, sem analysis coating surface has formed continuous, fine and close Al
2O
3And SiO
2Mixed oxide layer, thus the diffusion of oxygen to matrix successfully stoped.
By not comparing with preparing coating of material preparing cated matrix, its unit are weightening finish has reduced about 40mg/cm
2, prove that the cated matrix of preparation has good high-temperature oxidation resistant effect.