CN112645385B - YSZ/graphene composite powder for sealing coating and preparation method thereof - Google Patents
YSZ/graphene composite powder for sealing coating and preparation method thereof Download PDFInfo
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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Abstract
The invention relates to YSZ/graphene composite powder for a sealing coating and a preparation method thereof, belonging to the technical field of sealing coating materials. The composite powder is a fused eutectic composite powder composed of YSZ and graphene according to a mass ratio of 26-82: 1, and the YSZ is doped with the graphene, so that on one hand, the composite powder plays roles of a toughening phase and a pore-forming phase, and is beneficial to improving the overall toughness and wear resistance of the sealing coating, on the other hand, the composite powder can weaken the volume change caused by crystal form transformation of the YSZ, and is beneficial to enhancing the thermal stability of the sealing coating. The YSZ/graphene composite powder prepared by adopting the spray granulation and induction plasma spheroidizing process is simple to operate, is favorable for realizing densification, homogenization and spheroidization of the composite powder, and meets the requirement of preparing a sealing coating by adopting plasma spraying.
Description
Technical Field
The invention relates to YSZ/graphene composite powder for a sealing coating and a preparation method thereof, belonging to the technical field of sealing coating materials.
Background
With the development of aviation turbine engines in the direction of high flow ratio, high thrust-weight ratio and high inlet temperature, improving the working efficiency of the engines becomes the popular direction in current aviation engine research. Research shows that blade tip clearance has important influence on the efficiency of a compressor and a turbine, the power of an engine and the oil consumption rate. The clearance is too large, so that surging can be caused; if the clearance is too small, the moving and static parts in rotation may rub against each other. The sealing coating technology is one of the commonly used effective methods for reducing gaps, buffering dry friction and avoiding damaging blades. Therefore, the sealing coating needs to have good wear resistance, oxidation resistance, heat resistance, moderate hardness and strong bonding strength.
To meet the performance requirements described above, the seal coat is generally composed of a base phase, a lubricating phase and pores. At present, the working temperature of an engine reaches over 1200 ℃, and great challenges are caused to the high-temperature hot corrosion and the structural stability of the coating. Yttria partially stabilized zirconia (YSZ) is an ideal high-temperature resistant material, and has excellent characteristics of high melting point (2953K), small heat conduction, high hardness, good elasticity, high toughness, thermal shock resistance, oxidation resistance, corrosion resistance, good stability and the like, but when the temperature exceeds 1200 ℃, the YSZ is easy to generate phase change and sintering, so that the YSZ coating fails. Therefore, the development of a new sealing coating material is urgently needed to meet the sealing requirement of the high-temperature section of the engine.
Disclosure of Invention
Aiming at the defects in the prior art, the YSZ/graphene composite powder for the sealing coating and the preparation method thereof are provided, the composite powder of a melting eutectic state is obtained by doping nano YSZ with graphene, and the composite powder has good fluidity, compactness, wear resistance and high-temperature thermal stability, and meets the use requirement of the sealing coating in a high-temperature environment; in addition, the process for preparing the composite powder by adopting the spray granulation and induction plasma spheroidization processes is simple and is easy to realize large-scale production.
The purpose of the invention is realized by the following technical scheme.
The YSZ/graphene composite powder for the sealing coating is a molten eutectic state and consists of YSZ and graphene according to a mass ratio of 26-83: 1.
Further, the particle diameter of the composite powder is preferably 10 to 60 μm.
The invention discloses a preparation method of YSZ/graphene composite powder for a sealing coating, which comprises the following specific steps:
step 1, uniformly mixing nano YSZ powder, graphene, PVA (polyvinyl alcohol) and water to obtain turbid liquid;
step 2, transferring the turbid liquid to a spray drying granulation tower for agglomeration granulation, drying the granulated powder, and screening by a test sieve to obtain nano YSZ/graphene agglomerated powder with the particle size of 20-90 microns;
step 3, sending the nano YSZ/graphene agglomerated powder into an induction plasma spheroidizing device for spheroidizing, drying the spheroidized powder, and then screening by a test sieve to obtain YSZ/graphene composite powder for the sealing coating;
the induction plasma spheroidization parameters were as follows: the power is 40kW, the argon flow is 50 SCFH-60 SCFH, the hydrogen flow is 5 SCFH-6 SCFH, and the powder feeding rate is 4.0 RPM.
Furthermore, the particle size of the nano YSZ powder in the step 1 is preferably 400nm to 600 nm.
Further, mixing in a ball milling mode in the step 1 to obtain a suspension, wherein the ball milling rotation speed is 150 r/min-420 r/min, the ball milling time is 3 h-6 h, and the ball-material ratio is 3-5: 1.
Further, in the suspension obtained in the step 1, the mass percent of the PVA is 0.19-0.54%, and the sum of the mass percent of the nano YSZ powder and the mass percent of the graphene is 39-65%.
Further, the spray drying granulation process parameters in step 2 are as follows: the inlet temperature is 210-350 ℃, the outlet temperature is 100-150 ℃, the rotating speed of the spray head is 25-45 Hz, and the rotating speed of the peristaltic pump is 35-50 rpm.
Furthermore, the powder granulated in the step 2 is dried for 20 to 30 hours at the temperature of between 80 and 150 ℃.
Further, drying the spheroidized powder at 80-150 ℃ for 20-30 h.
Has the advantages that:
(1) the YSZ/graphene composite powder has the characteristics of melting recrystallization, compact combination of organization structures, good component uniformity, high sphericity and high fluidity, and meets the requirements of plasma spraying;
(2) according to the invention, the graphene is doped with YSZ, so that on one hand, the effects of a toughening phase and a pore-forming phase are achieved, the toughness and the wear resistance of the whole material are improved, on the other hand, the volume change caused by the crystal form transformation of YSZ can be weakened, the thermal stability of a sealing coating can be enhanced, and the sealing requirement of a gas path at a high-temperature section of an engine can be met;
(3) the preparation method of the YSZ/graphene composite powder by adopting the spray granulation and induction plasma spheroidizing process is simple to operate, is beneficial to realizing densification, homogenization and spheroidization of the composite powder, meets the requirement of preparing a sealing coating by adopting plasma spraying, and has good application prospect.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of the low power surface of the YSZ/graphene composite powder prepared in example 1.
Fig. 2 is a high-power surface scanning electron microscope image of the YSZ/graphene composite powder prepared in example 1.
Fig. 3 is a cross-sectional scanning electron microscope image of the nano YSZ/graphene agglomerated powder prepared in example 1.
Fig. 4 is a cross-sectional scanning electron microscope image of the YSZ/graphene composite powder prepared in example 1.
Fig. 5 is an X-ray diffraction (XRD) pattern of the YSZ/graphene composite powder prepared in example 1.
Fig. 6 is an elemental analysis diagram of the YSZ/graphene composite powder prepared in example 1.
Detailed Description
The present invention is further illustrated by the following detailed description, wherein the processes are conventional unless otherwise specified, and the starting materials are commercially available from a public source without further specification.
In the following examples:
and (4) SEM characterization: the morphology of the YSZ/graphene composite powder prepared in the examples and the morphology of the coating prepared in the examples were observed by a cold field emission scanning electron microscope, model S-4800, high and new technology, Japan.
XRD analysis: the X-ray diffraction spectrum of the X' PertPROMPD type polycrystalline X-ray diffraction manufactured by PANALYTICAL CORPORATION, the NetherlandsThe analyzer analyzes the YSZ/graphene composite powder prepared in the embodiment; and (3) testing conditions are as follows: k of CuαThe beam, Ni filter, tube voltage 40kV, tube current 40mA, slit size DS 0.957 °, PSD 2.12, and scanning speed 4 °/min.
And (3) testing the fluidity: the fluidity of the prepared YSZ/graphene composite powder was detected by using a FL4-1 Hall flowmeter manufactured by Beijing Steel research institute.
Spray drying prilling tower: LGZ-8 centrifugal spray dryer of Wuxi Dongjiang spray granulation drying machinery factory.
Induction plasma spheroidization equipment: induction Plasma spheroidizing equipment manufactured by TEKNA Plasma Systems inc.
PVA: the purity is more than or equal to 97 percent and is produced by Beijing Yili fine chemicals GmbH.
Nano YSZ: particle size 500nm, purity 99.9%, Kingjin research New Material science and technology Co., Ltd.
Preparing a coating: preparing a YSZ/graphene coating with the thickness of 0.1mm on a substrate from the composite powder prepared in the embodiment by adopting an atmospheric plasma spraying process; wherein the spraying distance is 80mm, the current is 900A, the flow rate of main gas (argon) is 90L/min, the flow rate of auxiliary gas (helium) is 40L/min, the flow rate of carrier gas (argon) is 8L/min, and the powder feeding rate is 4 RPM.
Characterization of the coating: selecting corundum with the nominal size of 100 meshes as an abrasive, wherein the amount of sand used is 20g each time, the erosion angle is 90 degrees, and carrying out an erosion abrasion experiment on the prepared coating; the impact wear resistance of the sample is evaluated by using the abrasion weight loss corresponding to the abrasive material of unit mass, and the smaller the weight loss is, the higher the impact wear resistance of the sample is.
Example 1
Step 1, adding 964g of nano YSZ powder, 36g of graphene, 5g of PVA and 1500g of deionized water into a ball milling tank, wherein the ball-material ratio is 4:1, and carrying out ball milling for 6 hours at the ball milling rotating speed of 150r/min to uniformly mix all the components to obtain a suspension;
step 2, transferring the turbid liquid to a spray drying granulation tower for agglomeration granulation, putting the granulated powder into an oven at 80 ℃ for drying for 30 hours, and then sieving to obtain nano YSZ/graphene agglomerated powder with the particle size of 20-90 microns;
wherein, the spray drying granulation process parameters are as follows: the inlet temperature is 240 ℃, the outlet temperature is 130 ℃, the rotating speed of the spray head is 35Hz, and the rotating speed of the peristaltic pump is 35 rpm;
step 3, sending the nano YSZ/graphene agglomerated powder into an induction plasma spheroidizing device for spheroidizing, drying the spheroidized powder in a drying oven at 100 ℃ for 30 hours, and then screening by using a test sieve to obtain YSZ/graphene composite powder with the particle size of 10-60 microns;
the induction plasma spheroidization parameters are as follows: the power is 40kW, the argon flow is 50SCFH, the hydrogen flow is 5SCFH, and the powder feeding rate is 4.0 RPM.
As can be seen from FIGS. 1 and 2, the prepared composite powder is spherical with a dense and smooth surface and a particle size distribution of 10 μm to 60 μm. Comparing fig. 3 and fig. 4, it can be seen that the nano YSZ/graphene agglomerated powder is spheroidized to form a fused eutectic composite powder, which has no obvious defects such as pores and cracks inside and is more compact in combination. YSZ and ZrO appear in XRD spectrogram of FIG. 42The characteristic peak of (A) indicates that the prepared composite powder is mainly YSZ. The element distribution characterization result of fig. 5 shows that the prepared composite powder has no obvious element segregation phenomenon. Tests show that the fluidity of the prepared composite powder is 70s/50 g.
The composite powder prepared by the embodiment is prepared into a YSZ/graphene coating with the thickness of 0.1mm on a nickel-based high-temperature alloy 3536 substrate by adopting an atmospheric plasma spraying process. The prepared coating is almost free of cracks, a small amount of gaps exist, the coating is compact, and the relative weight loss of the prepared coating is 6.53x10-4Far lower than x10 for conventional seal coating-3The magnitude indicates that the addition of the graphene plays a role in enhancing the erosion resistance of the sealing coating.
Example 2
Step 1, adding 976g of nano YSZ powder, 24g of graphene, 5g of PVA and 1500g of deionized water into a ball milling tank, wherein the ball-material ratio is 4:1, and carrying out ball milling for 3 hours at a ball milling rotating speed of 420r/min to uniformly mix all the components to obtain a suspension;
step 2, transferring the turbid liquid to a spray drying granulation tower for agglomeration granulation, putting the granulated powder into a drying oven at 150 ℃ for drying for 20 hours, and then sieving to obtain nano YSZ/graphene agglomerated powder with the particle size of 20-90 microns;
wherein, the spray drying granulation process parameters are as follows: the inlet temperature is 250 ℃, the outlet temperature is 140 ℃, the rotating speed of the spray head is 40Hz, and the rotating speed of the peristaltic pump is 35 rpm;
step 3, sending the nano YSZ/graphene agglomerated powder into an induction plasma spheroidizing device for spheroidizing, drying the spheroidized powder in a drying oven at 100 ℃ for 30 hours, and then screening by using a test sieve to obtain YSZ/graphene composite powder with the particle size of 10-60 microns;
the induction plasma spheroidization parameters are as follows: the power is 40kW, the argon flow is 55SCFH, the hydrogen flow is 6SCFH, and the powder feeding rate is 4.0 RPM.
According to the SEM characterization result, the composite powder prepared by the embodiment is a molten eutectic spherical powder, the surface is compact and smooth, no obvious defects such as holes and cracks exist in the composite powder, the combination is compact, and the particle size distribution is 10-60 microns. As can be seen from the test, the fluidity of the prepared composite powder is 78s/50 g.
The composite powder prepared by the embodiment is prepared into a YSZ/graphene coating with the thickness of 0.1mm on a nickel-based high-temperature alloy 3536 substrate by adopting an atmospheric plasma spraying process. The prepared coating is almost free of cracks, a small amount of gaps exist, the coating is compact, and the relative weight loss of the prepared coating is 7.81x10-4Far lower than x10 for conventional seal coating-3The magnitude indicates that the addition of the graphene plays a role in enhancing the erosion resistance of the sealing coating.
Example 3
Step 1, adding 988g of nano YSZ powder, 12g of graphene, 5g of PVA and 1500g of deionized water into a ball milling tank, wherein the ball-material ratio is 4:1, and carrying out ball milling for 3 hours at the ball milling rotating speed of 420r/min to uniformly mix all the components to obtain a suspension;
step 2, transferring the turbid liquid to a spray drying granulation tower for agglomeration granulation, putting the granulated powder into a drying oven at 150 ℃ for drying for 20 hours, and then sieving to obtain nano YSZ/graphene agglomerated powder with the particle size of 20-90 microns;
wherein, the spray drying granulation process parameters are as follows: the inlet temperature is 260 ℃, the outlet temperature is 150 ℃, the rotating speed of the spray head is 40Hz, and the rotating speed of the peristaltic pump is 40 rpm;
step 3, sending the nano YSZ/graphene agglomerated powder into an induction plasma spheroidizing device for spheroidizing, drying the spheroidized powder in a drying oven at 100 ℃ for 30 hours, and then screening by using a test sieve to obtain YSZ/graphene composite powder with the particle size of 10-60 microns;
the induction plasma spheroidization parameters are as follows: the power is 40kW, the argon flow is 60SCFH, the hydrogen flow is 6SCFH, and the powder feeding rate is 4.0 RPM.
According to the SEM characterization result, the composite powder prepared by the embodiment is a molten eutectic spherical powder, the surface is compact and smooth, no obvious defects such as holes and cracks exist in the composite powder, the combination is compact, and the particle size distribution is 10-60 microns. As can be seen from the test, the fluidity of the prepared composite powder is 87s/50 g.
The composite powder prepared by the embodiment is prepared into a YSZ/graphene coating with the thickness of 0.1mm on a nickel-based high-temperature alloy 3536 substrate by adopting an atmospheric plasma spraying process. The prepared coating has almost no cracks, a small amount of gaps exist, the coating is compact, and the relative weight loss of the prepared coating is 6.94x10-4Far lower than x10 for conventional seal coating-3The magnitude indicates that the addition of the graphene plays a role in enhancing the erosion resistance of the sealing coating.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The YSZ/graphene composite powder for the sealing coating is characterized in that: the composite powder is a molten eutectic state and is composed of YSZ and graphene according to the mass ratio of 26-83: 1;
the composite powder is prepared by the following method:
step 1, uniformly mixing nano YSZ powder, graphene, PVA and water to obtain turbid liquid;
step 2, transferring the turbid liquid to a spray drying granulation tower for agglomeration granulation, drying the granulated powder, and screening by a test sieve to obtain nano YSZ/graphene agglomerated powder with the particle size of 20-90 microns;
step 3, sending the nano YSZ/graphene agglomerated powder into an induction plasma spheroidizing device for spheroidizing, drying the spheroidized powder, and then screening by a test sieve to obtain YSZ/graphene composite powder for the sealing coating;
the induction plasma spheroidization parameters were as follows: the power is 40kW, the argon flow is 50 SCFH-60 SCFH, the hydrogen flow is 5 SCFH-6 SCFH, and the powder feeding rate is 4.0 RPM.
2. The YSZ/graphene composite powder for the seal coating of claim 1, which is characterized in that: the particle size of the composite powder is 10-60 mu m.
3. The YSZ/graphene composite powder for the seal coating of claim 1, which is characterized in that: the grain diameter of the nano YSZ powder in the step 1 is 400 nm-600 nm.
4. The YSZ/graphene composite powder for the seal coating of claim 1, which is characterized in that: and step 1, mixing in a ball milling mode to obtain a suspension, wherein the ball milling speed is 150-420 r/min, the ball milling time is 3-6 h, and the ball-to-material ratio is 3-5: 1.
5. The YSZ/graphene composite powder for the seal coating of claim 1, which is characterized in that: in the suspension obtained in the step 1, the mass percent of PVA is 0.19-0.54%, and the sum of the mass percent of nano YSZ powder and graphene is 39-65%.
6. The YSZ/graphene composite powder for the seal coating of claim 5, which is characterized in that: the spray drying granulation process parameters in step 2 are as follows: the inlet temperature is 210-350 ℃, the outlet temperature is 100-150 ℃, the rotating speed of the spray head is 25-45 Hz, and the rotating speed of the peristaltic pump is 35-50 rpm.
7. The YSZ/graphene composite powder for the seal coating of claim 1, which is characterized in that: and (3) drying the powder granulated in the step (2) at the temperature of between 80 and 150 ℃ for 20 to 30 hours.
8. The YSZ/graphene composite powder for the seal coating of claim 1, which is characterized in that: drying the spheroidized powder at 80-150 ℃ for 20-30 h.
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