CN107814589B - Method for in-situ coating of zirconium diboride-silicon carbide agglomerated powder by oxide - Google Patents
Method for in-situ coating of zirconium diboride-silicon carbide agglomerated powder by oxide Download PDFInfo
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Abstract
The invention relates to a method for in-situ coating of zirconium diboride-silicon carbide agglomerated powder by an oxide, belonging to the technical field of composite powder materials. The method is characterized in that the zirconium diboride-silicon carbide agglomerated powder is subjected to in-situ coating by using an oxide generated by autoxidation of the zirconium diboride-silicon carbide agglomerated powder in a high-temperature oxidation environment, and the composite powder with the core-shell structure is prepared. The oxide coated zirconium diboride-silicon carbide prepared by the method has high sphericity and density, and meets the requirements of plasma spraying on powder; the oxide coating layer generated by autoxidation can inhibit volatilization of silicon carbide in the plasma spraying process, loss of the silicon carbide is reduced, the melting point of the oxide is lower than that of zirconium boride, powder can be more sufficiently molten, the defects of gaps, vacancies and the like caused by overlapping of sheets in the coating are further filled, and the compactness of the coating is improved.
Description
Technical Field
The invention relates to preparation of zirconium diboride-silicon carbide core-shell structure powder, in particular to a method for realizing in-situ coating of zirconium diboride-silicon carbide agglomerated powder by using an oxide generated by autoxidation in a high-temperature oxidation environment, and belongs to the technical field of composite powder materials.
Background
The carbon fiber reinforced carbon matrix composite (C/C) has low density, low thermal expansion coefficient at high temperature and good mechanical property, is regarded as one of the most promising materials applied to hot-end parts of aircrafts, but is easily oxidized in an aerobic environment above 400 ℃ to cause the performance reduction, and the preparation of the oxidation-resistant ablation coating on the surface is one of effective methods.
Zirconium diboride (ZrB)2) Is a compound with a hexagonal metalloid structure and has the advantages of high melting point (3040 ℃), high hardness, excellent chemical stability and the like; silicon carbide (SiC) has the advantages of high strength, high hardness, low coefficient of thermal expansion, and the like. Therefore, the oxidation resistance of the composite coating prepared by adding silicon carbide into the zirconium diboride as a coating material can be effectively improved.
At present, the method for preparing micron agglomerated powder for zirconium diboride-silicon carbide plasma spraying mainly comprises ball milling powder mixing and spray granulation processes. The powder obtained by the process is not calcined and densified, the surface of the spherical powder is generally loose and rough, the strength is low, and the powder is easy to break and difficult to melt during conveying in the coating preparation process; and the anti-oxidation ablative coating prepared by utilizing the atmospheric plasma spraying system has the problems of more gaps, loose structure and the like. In view of this, there is an urgent need to develop a method for preparing composite zirconium diboride-silicon carbide powder suitable for ion spraying, so as to overcome the above disadvantages and meet the coating preparation requirements.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for coating zirconium diboride-silicon carbide agglomerated powder by oxide in situ, which has simple process and is suitable for industrial popularization; the prepared oxide coated zirconium diboride-silicon carbide with the core-shell structure has high sphericity and density, and meets the requirements of plasma spraying on powder; the oxide coating layer generated by autoxidation can inhibit volatilization of silicon carbide in the plasma spraying process, loss of the silicon carbide is reduced, the melting point of the oxide is lower than that of zirconium boride, powder can be more sufficiently molten, the defects of gaps, vacancies and the like caused by overlapping of sheets in the coating are further filled, and the compactness of the coating is improved.
The purpose of the invention is realized by the following technical scheme.
A method for in-situ coating of zirconium diboride-silicon carbide agglomerated powder by an oxide comprises the following steps:
step 1, uniformly mixing zirconium diboride, silicon carbide, polyvinyl alcohol (PVA) and absolute ethyl alcohol to obtain suspension;
in the suspension, the mass percent of the binder polyvinyl alcohol is 0.24-0.55%, the sum of the mass percent of zirconium diboride and silicon carbide is 35-60%, and the mass ratio of zirconium diboride to silicon carbide is 3-5: 1;
preferably, mixing by adopting a ball milling mode, carrying out ball milling for 2-6 h at the speed of 100-400 r/min, wherein the ball-material ratio is 3-5: 1, and uniformly mixing all the components to obtain a suspension;
step 2, transferring the suspension into a spray drying granulation tower for agglomeration granulation, drying the granulated powder, and screening to obtain zirconium diboride-silicon carbide agglomerated powder with the particle size of 20-90 microns;
wherein, the spray drying granulation parameters are as follows: the inlet temperature is 210-350 ℃, the outlet temperature is 100-130 ℃, the rotating speed of the spray head is 25-45 Hz, and the rotating speed of the peristaltic pump is 35-50 rpm;
preferably, drying at 80-150 ℃ for 20-30 h;
step 3, conveying the zirconium diboride-silicon carbide agglomerated powder into an atmosphere plasma spheroidizing device for spheroidizing, drying the spheroidized powder and screening by a test sieve to obtain spheroidized zirconium diboride-silicon carbide powder with the particle size of 10-60 mu m;
wherein, the atmospheric plasma spheroidization parameters are as follows: the flow rate of main gas (argon) is 85 SCFH-95 SCFH, the flow rate of auxiliary gas (helium) is 50 SCFH-60 SCFH, the flow rate of carrier gas (argon) is 10 SCFH-15 SCFH, the current is 900A-1000A, the powder feeding rate is 1.5 RPM-2.5 RPM, and the distance between spray guns is 45 mm-55 mm;
preferably, drying at 80-200 ℃ for 20-30 h;
and 4, placing the spheroidized zirconium diboride-silicon carbide powder in a tube furnace with oxygen, preserving the heat for 1 to 3 hours at the temperature of between 800 and 1000 ℃, and carrying out in-situ autoxidation reaction on the surface of the zirconium diboride-silicon carbide to generate an oxide coating layer so as to obtain the oxide coated zirconium diboride-silicon carbide powder with the core-shell structure.
Preferably, the flow rate of the oxygen in the tube furnace is 50 mL-150 mL/min.
Has the advantages that:
(1) the invention provides a method for in-situ coating zirconium diboride-silicon carbide agglomerated powder by using oxide, which is used for preparing a powder material with a core-shell structure, wherein the shell component is ZrO2A predominantly oxide with a core component of ZrB2a/SiC composite powder; the shell and the core are well combined, are compact and have certain bonding strength, and the method can improve the density and the cohesion of the powder and meet the requirement of plasma spraying.
(2) The core-shell structure powder material of zirconium diboride-silicon carbide in-situ coated by the oxide prepared by the method has the advantages that the melting point of the oxide generated by autoxidation is lower than that of zirconium boride, so that the powder can be more fully melted, the defects such as gaps and vacancies caused by lap joint of sheets in the coating can be filled in the process of preparing the coating, and the compactness of the coating is improved; and an oxide shell layer formed by autoxidation can inhibit volatilization of silicon carbide in the plasma spraying process, so that loss of the silicon carbide is reduced.
Drawings
Fig. 1 is a surface Scanning Electron Microscope (SEM) image of the oxide-coated zirconium diboride-silicon carbide powder prepared in example 1.
Fig. 2 is a cross-sectional Scanning Electron Microscope (SEM) image of the oxide-coated zirconium diboride-silicon carbide powder prepared in example 1.
Fig. 3 is an X-ray diffraction (XRD) pattern of the oxide-coated zirconium diboride-silicon carbide powder prepared in example 1.
FIG. 4 is a scanning electron microscope cross-sectional view of the coating prepared in example 1.
Detailed Description
The present invention is further illustrated by the following examples, wherein the processes are conventional unless otherwise specified, and the starting materials are commercially available from a public perspective unless otherwise specified.
In the following examples:
and (4) SEM characterization: observing the morphology of the oxide-coated zirconium diboride-silicon carbide powder prepared in the embodiment and the morphology of the prepared coating by using a cold field emission scanning electron microscope of Japanese high and new technology corporation S-4800;
x-ray diffraction analysis: the oxide-coated zirconium diboride-silicon carbide prepared in the examples was analyzed by an X' Pert PRO MPD type polycrystalline X-ray diffraction analyzer produced by PANALYtical, Netherlands; and (3) testing conditions are as follows: k of CuαRay, Ni filter, tube voltage 40kv, tube current 40mA, slit size DS 0.957 degree, PSD 2.12 degree, scanning speed 4 degree/min;
spray drying prilling tower: an LGZ-8 centrifugal spray dryer of a Wuxi Dongjiang spray granulation drying machinery plant;
atmosphere plasma spheroidizing equipment: the atmospheric plasma spray gun system described in "method for controlling atmosphere plasma spraying of easily oxidized coating in atmospheric open environment" reported in patent No. cn201410320466.
PVA: the purity is more than or equal to 97 percent and is produced by Beijing Yili fine chemicals GmbH.
ZrB is coated on the oxide prepared in the example by adopting a plasma spraying process2ZrB with the thickness of 0.2mm is prepared from-SiC powder2-a SiC coating; wherein, the spraying distance is 65mm, the current is 950A, the flow of main gas (argon) is 90SCFH, the flow of auxiliary gas (helium) is 55SCFH, the flow of carrier gas (argon) is 30SCFH, and the powder feeding rate is 2.0 RPM.
Example 1
(1) Adding 75g of zirconium diboride, 25g of silicon carbide, 0.8g of PVA and 100g of absolute ethyl alcohol into a ball milling tank, wherein the ball-to-material ratio is 4:1, and carrying out ball milling for 6 hours at 100r/min to uniformly mix all the components to obtain a suspension of precursor powder;
(2) transferring the suspension obtained in the step (1) to a spray drying granulation tower for agglomeration granulation, putting the granulated powder into an oven at 80 ℃ for drying for 30h, and then screening by a test sieve to obtain ZrB with the particle size of 20-90 mu m2-SiC agglomerated powder;
wherein, the spray drying granulation parameters are as follows: the inlet temperature is 210 ℃, the outlet temperature is 100 ℃, the rotating speed of the spray head is 25Hz, and the rotating speed of the peristaltic pump is 35 rpm;
(3) ZrB obtained in the step (2)2Sending the-SiC agglomerated powder into an atmosphere plasma spheroidizing device for spheroidizing, collecting the spheroidized powder by deionized water, drying the collected powder in a drying oven at 100 ℃ for 30h, and screening by a test sieve to obtain spheroidized ZrB with the particle size of 10-60 mu m2-SiC powder;
wherein, the atmospheric plasma spheroidization parameters are as follows: the current is 900A, the flow of main gas (argon) is 90SCFH, the flow of auxiliary gas (helium) is 50SCFH, the flow of carrier gas (argon) is 10SCFH, the powder feeding rate is 2.0RPM, and the distance between spray guns is 50 mm;
(4) spheroidized ZrB obtained in the step (3)2Placing the-SiC powder in a tube furnace, introducing oxygen with the flow of 100mL/min, heating to 800 ℃, preserving heat for 2 hours, and placing the powder in ZrB2The surface of the-SiC is subjected to in-situ autoxidation reaction to generate an oxide coating layer, and the oxide coated ZrB with a core-shell structure is obtained2-SiC powder.
As can be seen from FIG. 1, the prepared composite powder with the core-shell structure is in a spherical shape with a compact and smooth surface, and the particle size distribution is 10 μm to 60 μm. As can be seen from FIG. 2, the cross section of the prepared composite powder has an obvious core-shell structure, and the shell layer and the core are well combined.
The X-ray diffraction pattern of the prepared composite powder is shown in fig. 3, and characteristic peaks of zirconium diboride, silicon carbide and zirconia appear, so that the zirconia is mainly used as the oxide shell component.
As can be seen from fig. 4, the coating prepared from the composite powder prepared in this example has almost no cracks, has a small amount of voids, and is dense.
Example 2
(1) Adding 80g of zirconium diboride, 20g of silicon carbide, 0.7g of PVA and 100g of absolute ethyl alcohol into a ball milling tank, wherein the ball-to-material ratio is 4:1, and carrying out ball milling for 2 hours at 400r/min to uniformly mix all the components to obtain a suspension of precursor powder;
(2) transferring the suspension obtained in the step (1)Carrying out agglomeration granulation in a spray drying granulation tower, putting the granulated powder into a drying oven at 150 ℃ for drying for 20h, and then carrying out inspection screening to obtain ZrB with the grain diameter of 20-90 mu m2-SiC agglomerated powder;
wherein, the spray drying granulation parameters are as follows: the inlet temperature is 350 ℃, the outlet temperature is 130 ℃, the rotating speed of the spray head is 45Hz, and the rotating speed of the peristaltic pump is 50 rpm;
(3) ZrB obtained in the step (2)2Sending the-SiC agglomerated powder into an atmosphere plasma spheroidizing device for spheroidizing, collecting the spheroidized powder by deionized water, drying the collected powder in a drying oven at 200 ℃ for 20h, and screening by a test sieve to obtain spheroidized ZrB with the particle size of 10-60 mu m2-SiC powder;
wherein, the atmospheric plasma spheroidization parameters are as follows: the current is 950A, the flow of main gas (argon) is 95SCFH, the flow of auxiliary gas (helium) is 50SCFH, the flow of carrier gas (argon) is 10SCFH, the powder feeding rate is 2.0RPM, and the distance between spray guns is 50 mm;
(4) spheroidized ZrB obtained in the step (3)2Placing the-SiC powder in a tube furnace, introducing oxygen with the flow of 60mL/min, heating to 1000 ℃, preserving heat for 1h, and placing the powder in ZrB2The surface of the-SiC is subjected to in-situ autoxidation reaction to generate an oxide coating layer, and the oxide coated ZrB with a core-shell structure is obtained2-SiC powder.
Performing SEM representation on the prepared composite powder, wherein the prepared composite powder is in a spherical shape with a compact and smooth surface and has a particle size distribution of 10-60 mu m according to a representation result; according to the cross section SEM representation result, the prepared composite powder has obvious core-shell structure, and the shell layer and the inner core are well combined. The XRD spectrogram of the prepared composite powder has characteristic peaks of zirconium diboride, silicon carbide and zirconium oxide, which shows that the components of the zirconia are mainly the zirconium oxide. The composite powder prepared by the embodiment can be used for preparing a crack-free and compact coating.
Example 3
(1) Adding 82g of zirconium diboride, 18g of silicon carbide, 0.9g of PVA and 100g of absolute ethyl alcohol into a ball milling tank, wherein the ball-to-material ratio is 4:1, and carrying out ball milling for 4 hours at 300r/min to uniformly mix all the components to obtain a suspension of precursor powder;
(2) transferring the suspension obtained in the step (1) to a spray drying granulation tower for agglomeration granulation, putting the granulated powder into a 120 ℃ oven for drying for 25h, and then screening by a test sieve to obtain ZrB with the particle size of 20-90 mu m2-SiC agglomerated powder;
wherein, the spray drying granulation parameters are as follows: the inlet temperature is 270 ℃, the outlet temperature is 120 ℃, the rotating speed of the spray head is 30Hz, and the rotating speed of the peristaltic pump is 40 rpm;
(3) ZrB obtained in the step (2)2Sending the-SiC agglomerated powder into an atmosphere plasma spheroidizing device for spheroidizing, collecting the spheroidized powder by deionized water, drying the collected powder in a drying oven at 150 ℃ for 25h, and screening by a test sieve to obtain spheroidized ZrB with the particle size of 10-60 mu m2-SiC powder;
wherein, the atmospheric plasma spheroidization parameters are as follows: the current 930A, the main gas (argon) flow rate of 92SCFH, the auxiliary gas (helium) flow rate of 57SCFH, the carrier gas (argon) flow rate of 12SCFH, the powder feeding rate of 2.3RPM and the spray gun distance of 55 mm;
(4) spheroidized ZrB obtained in the step (3)2Placing the-SiC powder in a tube furnace, introducing oxygen with the flow rate of 150mL/min, heating to 900 ℃, preserving heat for 3h, and placing the heated SiC powder in ZrB2The surface of the-SiC is subjected to in-situ autoxidation reaction to generate an oxide coating layer, and the oxide coated ZrB with a core-shell structure is obtained2-SiC powder.
Performing SEM representation on the prepared composite powder, wherein the prepared composite powder is in a spherical shape with a compact and smooth surface and has a particle size distribution of 10-60 mu m according to a representation result; according to the cross section SEM representation result, the prepared composite powder has obvious core-shell structure, and the shell layer and the inner core are well combined. The XRD spectrogram of the prepared composite powder has characteristic peaks of zirconium diboride, silicon carbide and zirconium oxide, which shows that the components of the zirconia are mainly the zirconium oxide. The composite powder prepared by the embodiment can be used for preparing a crack-free and compact 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 (5)
1. A method for coating zirconium diboride-silicon carbide agglomerated powder in situ by oxide is characterized by comprising the following steps: the steps of the method are as follows,
step 1, uniformly mixing zirconium diboride, silicon carbide, polyvinyl alcohol and absolute ethyl alcohol to obtain suspension; wherein the mass ratio of zirconium diboride to silicon carbide is 3-5: 1;
step 2, transferring the suspension into a spray drying granulation tower for agglomeration granulation, drying the granulated powder, and screening to obtain zirconium diboride-silicon carbide agglomerated powder with the particle size of 20-90 microns;
step 3, conveying the zirconium diboride-silicon carbide agglomerated powder into an atmosphere plasma spheroidizing device for spheroidizing, drying the spheroidized powder and screening by a test sieve to obtain spheroidized zirconium diboride-silicon carbide powder with the particle size of 10-60 mu m;
and 4, placing the spheroidized zirconium diboride-silicon carbide powder in a tubular furnace with oxygen, wherein the flow rate of the oxygen in the tubular furnace is 50-150 mL/min, and preserving the heat for 1-3 h at 800-1000 ℃ to obtain the oxide coated zirconium diboride-silicon carbide powder with the core-shell structure.
2. The method for in-situ coating of zirconium diboride-silicon carbide agglomerated powder by oxide according to claim 1, wherein the method comprises the following steps: in the suspension liquid in the step 1, the mass percent of the polyvinyl alcohol is 0.24-0.55%, and the sum of the mass percent of the zirconium diboride and the mass percent of the silicon carbide is 35-60%.
3. The method for in-situ coating of zirconium diboride-silicon carbide agglomerated powder by oxide according to claim 1, wherein the method comprises the following steps: and step 1, mixing by adopting a ball milling mode, carrying out ball milling for 2-6 h at the speed of 100-400 r/min, wherein the ball-material ratio is 3-5: 1, and uniformly mixing all the components to obtain a suspension.
4. The method for in-situ coating of zirconium diboride-silicon carbide agglomerated powder by oxide according to claim 1, wherein the method comprises the following steps: the parameters of spray drying granulation in the step 2 are as follows: the inlet temperature is 210-350 ℃, the outlet temperature is 100-130 ℃, the rotating speed of the spray head is 25-45 Hz, and the rotating speed of the peristaltic pump is 35-50 rpm.
5. The method for in-situ coating of zirconium diboride-silicon carbide agglomerated powder by oxide according to claim 1, wherein the method comprises the following steps: the atmospheric plasma spheroidization parameters in the step 3 are as follows: the main gas flow is 85 SCFH-95 SCFH, the auxiliary gas flow is 50 SCFH-60 SCFH, the carrier gas flow is 10 SCFH-15 SCFH, the current is 900A-1000A, the powder feeding rate is 1.5 RPM-2.5 RPM, the spray gun distance is 45 mm-55 mm, the main gas and the carrier gas are argon, and the auxiliary gas is helium.
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| CN109437911A (en) * | 2018-12-04 | 2019-03-08 | 合肥睿涌陶瓷材料科技有限公司 | A kind of flame heat spray carbide composite ceramic stick and preparation method thereof |
| CN112194506A (en) * | 2020-08-26 | 2021-01-08 | 北京理工大学 | Preparation of oxide in-situ coated ZrB by using oxyacetylene fuel flow2Method for agglomerating powder by using-SiC |
| CN113248261B (en) * | 2021-06-16 | 2022-05-10 | 北京理工大学 | Molybdenum disilicide coated tantalum boride-hafnium carbide spherical powder and preparation method thereof |
| CN113880586B (en) * | 2021-07-29 | 2022-12-13 | 北京理工大学 | Hafnium diboride-tantalum disilicide composite powder and preparation method thereof |
| CN116425566B (en) * | 2023-04-26 | 2024-07-12 | 北京理工大学 | LaSi 2-modified ZrB 2-SiC-doped composite powder and preparation method thereof, and thermal protection coating and preparation method thereof |
| CN117026154B (en) * | 2023-07-19 | 2024-09-27 | 北京金轮坤天特种机械有限公司 | Preparation method of zirconium diboride compact coating |
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| CN101560103B (en) * | 2009-05-27 | 2012-01-25 | 哈尔滨工业大学 | Method for in situ generating film with high oxidation resistance on surface of zirconium boride-silicon carbide ceramic composite material |
| CN101747047B (en) * | 2009-10-21 | 2012-07-18 | 哈尔滨工业大学 | Method for improving heat shock resistance and strength of ZrB2-SiC superhigh temperature ceramic material |
| CN103422046B (en) * | 2013-08-20 | 2015-11-04 | 航天材料及工艺研究所 | The preparation method of a kind of zirconium diboride-silicon carbide high-temperature oxidation resistant coating |
| CN103601192B (en) * | 2013-11-12 | 2015-07-08 | 北京理工大学 | Preparation method of spherical zirconium diboride and silicon carbide aggregate powder |
| CN104557050B (en) * | 2014-12-20 | 2017-02-22 | 北京矿冶研究总院 | ZrB 2-SiC/Si composite powder with core-shell structure and preparation method thereof |
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