CN115894034A - Preparation method of chromium aluminum carbide ceramic, chromium aluminum carbide ceramic and application - Google Patents
Preparation method of chromium aluminum carbide ceramic, chromium aluminum carbide ceramic and application Download PDFInfo
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- QRRWWGNBSQSBAM-UHFFFAOYSA-N alumane;chromium Chemical compound [AlH3].[Cr] QRRWWGNBSQSBAM-UHFFFAOYSA-N 0.000 title claims abstract description 97
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- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 5
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- QQHSIRTYSFLSRM-UHFFFAOYSA-N alumanylidynechromium Chemical compound [Al].[Cr] QQHSIRTYSFLSRM-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
The application relates to a preparation method of chromium aluminum carbide ceramic, chromium aluminum carbide ceramic and application, and belongs to the technical field of ceramic material preparation. The preparation method of the chromium aluminum carbide ceramic comprises the following steps: s1, carrying out ball-milling pretreatment on chromium powder; s2, aluminum powder, carbon powder and chromium powder obtained by the ball milling treatment are mixed according to the molar ratio (1-1.1): 1:2, ball milling after mixing to obtain mixed powder; s3, sintering the mixed powder under a protective atmosphere or vacuum condition to obtain a precursor; s4, crushing the precursor, and ball-milling the crushed precursor, the solvent, the binder and the dispersant to obtain slurry; and S5, adjusting the pH value of the slurry to be alkaline, and then performing spray granulation to obtain the chromium aluminum carbide ceramic. The preparation method of the chromium aluminum carbide ceramic can improve the sphericity, the fluidity, the purity, the thermal shock resistance and the high-temperature corrosion resistance of the chromium aluminum carbide ceramic powder, further reduce the preparation difficulty of the chromium aluminum carbide coating and improve the preparation efficiency and the quality of the coating.
Description
Technical Field
The invention relates to the technical field of ceramic material preparation, in particular to a preparation method of chromium aluminum carbide ceramic, the chromium aluminum carbide ceramic and application.
Background
Ternary layered ceramic (M) n+1 AX n Phase or MAX phase) belonging to a layered hexagonal structure, wherein "M" represents an early transition group metal element, "a" represents a main group element (mostly group IIIA and IVA elements), and "X" represents C or N. In the crystal structure of the material, M layers which are close to each other and are closely packed are staggered with pure A element layers, and X atoms are filled in octahedral positions among the M layers, namely transition metal carbonitride M n+1 X n The nano-sheet layer and the A-group atomic layer are stacked in a staggered mode. Due to the unique structural characteristics, the MAX phase compound has excellent comprehensive performance, not only has the characteristics of low density, high melting point, high elastic modulus, high yield strength and the like of the traditional ceramic material, but also has the properties of electric conduction and heat conduction of a metal material, good microscopic plasticity, easiness in machining, high damage tolerance and the like; the weak metallic bonds between the layered structures provide the MAX phase compounds with self-lubricity properties superior to that of graphite. Therefore, the ceramic can be used as a connecting material between metal and ceramic, a high-temperature precise structure material, an electrode material or an anti-corrosion coating and the like, and is a novel functional structure ceramic.
Chromium aluminium carbide (Cr) 2 AlC) as a typical representative of the ternary layered ceramic, has good high-temperature stability, high-temperature oxidation resistance, and thermal shock resistance due to its special element composition in addition to the above-described characteristics. Cr (chromium) component 2 A layer of Cr is generated on the surface of AlC in the high-temperature oxidation process 2 O 3 Under which is a layer of dense Al 2 O 3 Oxygen diffusion into the interior can be effectively blocked. Thus, cr is comparable to other ternary layered ceramics 2 AlC has better high-temperature oxidation resistance, and is widely researched as a high-temperature structure material, a high-temperature protective coating material and a high-temperature coating transition layer material at present.
At present, the high-temperature protective coating material and the high-temperature coating transition layer are mainly prepared by the methods of multi-arc ion plating, magnetron sputtering, thermal spraying and the like. However, cr prepared by conventional techniques 2 AlC ceramic powder having poor flowability, useThe coating prepared by the thermal spraying process has the advantages of more defects, poor compactness, poor thermal shock resistance, high requirement on equipment and high preparation cost of the coating.
Disclosure of Invention
Based on the above, there is a need to provide a preparation method of chromium aluminum carbide ceramic, chromium aluminum carbide ceramic and application thereof, so as to improve the sphericity, fluidity, purity, thermal shock resistance and high temperature corrosion resistance of the chromium aluminum carbide ceramic, further reduce the preparation difficulty of the chromium aluminum carbide coating, and improve the preparation efficiency and quality of the coating.
The specific technical scheme of the application is as follows:
in one aspect of the present application, a method for preparing chromium aluminum carbide ceramic is provided, which comprises the following steps:
s1, carrying out ball-milling pretreatment on chromium powder;
s2, aluminum powder, carbon powder and chromium powder obtained by the pre-ball milling treatment are mixed according to the molar ratio (1-1.1): 1:2, ball milling after mixing to obtain mixed powder;
s3, sintering the mixed powder under a protective atmosphere or vacuum condition to obtain a precursor;
s4, crushing the precursor, and ball-milling the crushed precursor, the solvent, the binder and the dispersant to obtain slurry;
and S5, adjusting the pH value of the slurry to be alkaline, and then carrying out spray granulation to obtain the chromium aluminum carbide ceramic.
In some embodiments, the slurry comprises, in mass percent: 10 to 20 percent of precursor, 1 to 2 percent of binder, 0.5 to 2 percent of dispersant and 78.5 to 86 percent of solvent.
In some embodiments, the chromium powder has a particle size of 325 to 800 mesh, the aluminum powder has a particle size of 200 to 400 mesh, and the carbon powder has a particle size of 325 to 800 mesh.
In some embodiments, the chrome powder obtained by the pre-ball milling has an average particle size D50 of 10 μm to 15 μm, and the mixed powder has an average particle size D50 of 12 μm to 16 μm.
In some embodiments, the protective atmosphere comprises one or more of an inert gas and nitrogen.
In some embodiments, the protective atmosphere comprises one or more of an inert gas comprising one or more of helium, neon, argon, krypton, and xenon, and nitrogen.
In some embodiments, the degree of vacuum for sintering is 1 × 10 -3 Pa～5×10 -3 Pa。
In some embodiments, the temperature ramp rate for the sintering is between 5 ℃/min and 10 ℃/min.
In some embodiments, the sintering temperature is 1050 ℃ to 1150 ℃.
In some embodiments, the sintering time is between 6h and 10h.
In some embodiments, the binder comprises one or more of polyvinyl alcohol, polystyrene, and hydroxymethylcellulose.
In some embodiments, the dispersant comprises ammonium polyacrylate.
In some embodiments, the solvent comprises one or more of water, ethanol, and acetone.
In some embodiments, the process conditions for spray granulation include: the diameter of the nozzle is 0.1 mm-3 mm, the air inlet temperature is 50-250 ℃, the air outlet temperature is 40-200 ℃, the rotation speed of the peristaltic pump is 20 r/min-80 r/min, and the rotation speed of the fan is 20 r/min-80 r/min.
In another aspect of the application, a chromium aluminum carbide ceramic is provided, which is prepared by the preparation method.
In some embodiments, the chromium aluminum carbide ceramic has a D10 of 4 to 8 μm, a D50 of 20 to 28 μm, a D90 of 35 to 42 μm, and a specific surface area of 400m 2 /kg～550m 2 Kg, bulk density of 0.957g/cm 3 ～1.527g/cm 3 。
In a further aspect of the present application, there is provided a chromium aluminum carbide ceramic prepared by the above preparation method or an application of the above chromium aluminum carbide ceramic in a thermal spraying process.
In some embodiments, the thermal spray process is used to form the chromium aluminum carbide ceramic into a high temperature protective coating, a high temperature coating transition layer, or a corrosion resistant coating.
Compared with the prior art, the preparation method of the chromium aluminum carbide ceramic, the chromium aluminum carbide ceramic and the application have at least the following advantages:
(1) The precursor is sintered under a protective atmosphere or vacuum condition and then prepared into slurry for spray granulation, so that pressurization before or in the process of sintering chromium aluminum carbide into a phase is avoided, the phase forming process is simple, the operation is convenient, mass production with low cost can be realized, the introduction of impurities in the granulation process can also be avoided, and high-purity-phase chromium aluminum carbide ceramic powder can be obtained.
(2) The preparation method of the chromium aluminum carbide ceramic is simple, the requirement on equipment is low, the chromium aluminum carbide high-purity powder with uniform granularity, high sphericity and good fluidity can be obtained after spray granulation, the technical requirements of various thermal spraying processes can be met, and the coating obtained after spraying has good integrity and high density.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a chromium aluminum carbide ceramic according to an embodiment of the present disclosure.
FIG. 2 is an X-ray diffraction pattern of the chromium aluminum carbide ceramic powder prepared in example 1 of the present application.
Fig. 3 is an SEM image of chromium aluminum carbide ceramic powder prepared in example 1 of the present application.
Fig. 4 is a cross-sectional SEM image of the chromium aluminum carbide ceramic powder prepared in example 1 of the present application.
Fig. 5 is a cross-sectional SEM image of a chromium aluminum carbide coating prepared in example 2 of the present application.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, as those skilled in the art will recognize without departing from the spirit and scope of the present invention.
In the description of the present invention, unless otherwise defined, terms of art and terminology not specifically described have the same meaning as commonly understood by those skilled in the art and are common general knowledge of those skilled in the art, and methods not specifically described are conventional methods well known to those skilled in the art. The term "plurality" in the present invention means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, the technical features described in the open type include a closed technical solution including the listed features, and also include an open technical solution including the listed features.
When the chromium aluminum carbide obtained by the traditional preparation method is used for a thermal spraying process, the obtained chromium aluminum carbide has poor fluidity, so that the thermal spraying process is influenced, and the application of the high-efficiency thermal spraying process cannot be realized. The traditional method also comprises the steps of dispersing MAX phase powder in a solvent to obtain slurry, and spraying the slurry from a nozzle by adopting a thermal spraying technology to prepare the coating, but the prepared coating has the defects of more defects, poor compactness and poor thermal shock resistance, is not suitable for a high-temperature chromium aluminum carbide protective coating with high compactness, has high requirements on equipment, and has high preparation cost of the coating. The conventional method also produces chromium aluminum carbide by pressing before or during phase formation, but only a small amount of chromium aluminum carbide can be synthesized at a very high cost each time. In view of this, the present application provides a preparation method of chromium aluminum carbide ceramic, chromium aluminum carbide ceramic and application thereof to solve the above technical problems.
Referring to fig. 1, an embodiment of the present application provides a method for preparing a chromium aluminum carbide ceramic, including the following steps:
s1, carrying out ball-milling pretreatment on chromium powder;
s2, aluminum powder, carbon powder and chromium powder obtained by the pre-ball milling treatment are mixed according to the molar ratio (1-1.1): 1:2, mixing and then performing ball milling to obtain mixed powder;
s3, sintering the mixed powder under a protective atmosphere or vacuum condition to obtain a precursor;
s4, crushing the precursor, and ball-milling the crushed precursor, the solvent, the binder and the dispersant to obtain slurry;
and S5, adjusting the pH value of the slurry to be alkaline, and then performing spray granulation to obtain the chromium aluminum carbide ceramic.
It can be understood that the molar ratio of the aluminum powder, the carbon powder and the chromium powder obtained by pre-ball milling can be 1:1:2. 1.01:1: 2. 1.02:1: 2. 1.03:1: 2. 1.05:1: 2. 1.07:1: 2. 1.09:1:2 or 1.1:1:2. it should be noted that the reason for performing spray granulation after adjusting the pH of the slurry to be weakly alkaline is that appropriate dispersants and binders are more soluble and stable in an alkaline environment, and the powder is more dispersible and stable in a weakly alkaline solution. The pH can be adjusted to 8 to 10, for example, the pH can be adjusted to 8, 8.5, 9, 9.5, or 10, and the like. The preparation method of the chromium aluminum carbide ceramic comprises the steps of sintering into the phase and then carrying out spray granulation, avoids pressurization before or during sintering of the chromium aluminum carbide into the phase, has simple phase forming process, simple process and convenient operation, can carry out mass production with low cost, avoids introducing impurities during granulation, and can obtain high-purity-phase chromium aluminum carbide (Cr) 2 AlC) ceramic powder, the chromium aluminum carbide ceramic powder prepared by the spray granulation has high sphericity and good fluidity, can meet the technical requirements of various thermal spraying processes, and can improve the integrity and the density of a coating obtained after spraying. Further, the chromium-aluminum carbide ceramic powder with more uniform granularity, higher sphericity and better fluidity can be obtained by screening powder grading.
In some embodiments, the step S1 of performing the ball milling treatment on the chromium powder is performed by wet ball milling. Specifically, grinding balls, chromium powder and a ball-milling medium solvent are mixed according to a weight ratio of 2:1: (1-1.6) adding the mixture into a ball milling tank, carrying out ball milling for 8-10 hours, and drying the chromium powder suspension obtained by ball milling in a vacuum oven to obtain the chromium powder subjected to ball milling treatment. Optionally, the milling media solvent comprises one or more of water, ethanol, and acetone; the drying temperature of the vacuum oven is 60-90 ℃, and the drying time is 2-3 h. It is understood that the weight ratio of the grinding ball, the chromium powder and the solvent of the ball milling medium can be 2:1: 1.2: 1:1.1, 2:1:1.2, 2:1:1.4 or 2:1:1.6; the ball milling time may be 8 hours, 8.5 hours, 9 hours, 9.5 hours, or 10 hours, and the ball milling time may be other values between 8 hours and 10 hours.
In some embodiments, the step S1 of performing the ball milling treatment on the chromium powder is performed by a dry ball milling method. Specifically, the grinding ball and the chromium powder are mixed according to the weight ratio (4-5): 1, ball milling for 9-12 hours in protective atmosphere after mixing to obtain the chromium powder after ball milling treatment. It will be appreciated that the weight ratio of the grinding ball to the chromium powder may be 4: 1. 4.1: 1. 4.2: 1. 4.3: 1. 4.4: 1. 4.6: 1. 4.8:1 or 5:1, etc.; the ball milling time can be 9 hours, 9.5 hours, 10 hours, 10.5 hours, 11 hours, 11.5 hours or 12 hours, and can also be other values between 9 hours and 12 hours; the protective atmosphere comprises one or more of inert gas and nitrogen; optionally, the inert gas comprises one or more of helium, neon, argon, krypton, and xenon.
In some embodiments, the aluminum powder, carbon powder, and pre-ball milled chromium powder are mixed and then wet ball milled. Specifically, aluminum powder, carbon powder and chromium powder obtained by pre-ball milling are mixed to form a mixed material, and the mixed material, the grinding balls and a ball milling medium solvent are mixed according to the weight ratio of 1:3: (1-1.6) adding the mixture into a ball milling tank, ball milling for 4-6 hours, and drying the mixed powder suspension obtained after ball milling in a vacuum oven to obtain the mixed powder. Optionally, the milling media solvent comprises one or more of water, ethanol, and acetone; the drying temperature of the vacuum oven is 60-90 ℃, and the drying time is 2-3 h. It is understood that the weight ratio of the mixing material, the grinding balls and the solvent of the ball milling medium may be 1:3: 1.1: 3:1.1, 1:3:1.2, 1:3:1.3, 1:3:1.4, 1:3:1.5 or 1:3:1.6; the ball milling time may be 4 hours, 4.5 hours, 5 hours, 5.5 hours, or 6 hours, and may be other values between 4 hours and 6 hours.
In some embodiments, the aluminum powder, carbon powder, and pre-ball milled chromium powder are mixed and then dry ball milled. Specifically, aluminum powder, carbon powder and chromium powder obtained by pre-ball milling are mixed to form a mixed material, and the mixed material and a grinding ball are mixed according to the weight ratio of 1: (4-5) ball milling for 5-8 hours in a protective atmosphere to obtain mixed powder. It will be appreciated that the weight ratio of the mixed material to the grinding balls may be 1: 4.1: 4.1, 1:4.2, 1:4.3, 1:4.4, 1:4.5, 1:4.7, 1:4.9 or 1:5; the ball milling time may be any value between 5 hours and 8 hours, and may be, for example, 5 hours, 5.5 hours, 6 hours, 6.5 hours, 7 hours, 7.5 hours, or 8 hours; the protective atmosphere comprises one or more of inert gas and nitrogen; optionally, the inert gas comprises one or more of helium, neon, argon, krypton, and xenon.
In some embodiments, the pre-ball milling process of step S1 and the ball milling process of step S2 use three grinding balls with diameters of 1mm to 3mm, 5mm to 7mm, and 8mm to 10mm, respectively, and the weight ratio of the three grinding balls is 1: (1-1.2): (1-1.2). It will be appreciated that the diameters of the three grinding balls may be 1mm, 5mm, 10mm, or 2mm, 5mm, 8mm, or 3mm, 7mm, 9mm, or 3mm, 6mm, 8mm, respectively; the weight ratio of the three grinding balls can be 1:1:1, or 1:1.1:1.2, or 1:1.2:1.1, or 1:1.1:1.1, etc.
In some embodiments, the wet ball milling in step S1 and step S2 uses a ball mill with a rotational speed of 350r/min to 400r/min, and the dry ball milling uses a ball mill with a rotational speed of 300r/min to 400r/min. It is understood that the ball mill rotation speed used in wet ball milling can be 350r/min, 355r/min, 360r/min, 365r/min, 370r/min, 375r/min, 380r/min, 385r/min, 390r/min, 395r/min, 400r/min, etc., and the ball mill rotation speed used in dry ball milling can be 350r/min, 353r/min, 356r/min, 360r/min, 365r/min, 368r/min, 370r/min, 375r/min, 380r/min, 382r/min, 385r/min, 390r/min, 395r/min, 400r/min, etc.
In some embodiments, the chromium powder has a particle size of 325 to 800 mesh, the aluminum powder has a particle size of 200 to 400 mesh, and the carbon powder has a particle size of 325 to 800 mesh. It is understood that the particle size of the chromium powder may be 325 mesh, 400 mesh, 500 mesh, 600 or 800 mesh, etc.; the particle size of the aluminum powder can be 200 meshes, 230 meshes, 270 meshes, 325 meshes, 400 meshes and the like; the particle size of the carbon powder (or graphite powder) can be 325 meshes, 400 meshes, 500 meshes, 600 meshes, 800 meshes or the like. In the present application, "-200 mesh" means that the particle size of the powder is not larger than the mesh size of a 200 mesh screen.
In some embodiments, the chrome powder obtained by pre-ball milling has an average particle diameter D50 of 10 μm to 15 μm, and the mixed powder has an average particle diameter D50 of 12 μm to 16 μm. The average particle diameter D50 of the chromium powder obtained by the preliminary ball milling may be 10 μm, 10.4 μm, 10.8 μm, 11 μm, 11.3 μm, 11.7 μm, 12 μm, 12.2 μm, 12.6 μm, 13 μm, 13.5 μm, 14 μm, 14.5 μm, 15 μm or the like; the average particle diameter D50 of the mixed powder may be 12 μm, 12.3 μm, 12.7 μm, 13 μm, 13.4 μm, 13.7 μm, 14 μm, 14.2 μm, 14.8 μm, 15 μm, 15.4 μm, 15.6 μm, 16 μm or the like. The chromium powder is subjected to the ball-milling pretreatment, so that the particle size range of the chromium powder subjected to the ball-milling pretreatment is effectively controlled, and the mass fraction of the effective components of the chromium powder subjected to the ball-milling pretreatment is improved.
In some embodiments, the protective atmosphere in step S3 comprises one or more of an inert gas and nitrogen.
In some embodiments, the protective atmosphere in step S3 comprises one or more of an inert gas and nitrogen, the inert gas comprising one or more of helium, neon, argon, krypton, and xenon.
In some embodiments, the degree of vacuum for sintering in step S3 is 1 × 10 -3 Pa～5×10 -3 Pa。
In some embodiments, the temperature rise rate for sintering in step S3 is from 5 ℃/min to 10 ℃/min. It is understood that the temperature increase rate of sintering may be any value between 5 ℃/min and 10 ℃/min, and for example, may be 5 ℃/min, 5.3 ℃/min, 5.8 ℃/min, 6 ℃/min, 6.3 ℃/min, 6.6 ℃/min, 7 ℃/min, 7.2 ℃/min, 7.6 ℃/min, 8 ℃/min, 8.3 ℃/min, 8.8 ℃/min, 9 ℃/min, 9.5 ℃/min, or 10 ℃/min.
In some embodiments, the temperature for sintering in step S3 is 1050 ℃ to 1150 ℃. It is understood that the sintering temperature may be 1050 deg.C, 1060 deg.C, 1070 deg.C, 1080 deg.C, 1090 deg.C, 1110 deg.C, 1120 deg.C, 1130 deg.C, 1140 deg.C or 1150 deg.C, or other values between 1050 deg.C and 1150 deg.C.
In some embodiments, the sintering time in step S3 is 6h to 10h. It is understood that the sintering time can be 6h, 6.2h, 6.5h, 6.7h, 7h, 7.3h, 7.5h, 7.8h, 8h, 8.2h, 8.5h, 8.8h, 9h, 9.4h, 9.7h or 10h, and the sintering time can be other values between 6h and 10h.
In some embodiments, the slurry comprises, in mass percent: 10 to 20 percent of precursor, 1 to 2 percent of binder, 0.5 to 2 percent of dispersant and 78.5 to 86 percent of solvent. It is understood that the slurry may include, in mass percent, 10% of the precursor, 1% of the binder, 0.5% of the dispersant, and 88.5% of the solvent, or may include 12% of the precursor, 1.5% of the binder, 0.5% of the dispersant, and 86% of the solvent, or may include 15% of the precursor, 2% of the binder, 1% of the dispersant, and 82% of the solvent, or may include 20% of the precursor, 2% of the binder, 2% of the dispersant, and 76% of the solvent, or may include 20% of the precursor, 1% of the binder, 0.5% of the dispersant, and 78.5% of the solvent.
In some embodiments, the binder comprises one or more of polyvinyl alcohol (PVA), polystyrene (PS), and hydroxymethylcellulose (CMC). It is understood that the binder may be any one of polyvinyl alcohol (PVA), polystyrene (PS) and hydroxymethyl cellulose (CMC), and may be a mixture of a plurality of polyvinyl alcohol (PVA), polystyrene (PS) and hydroxymethyl cellulose (CMC) in any ratio.
In some embodiments, the dispersant comprises ammonium polyacrylate.
In some embodiments, the solvent comprises one or more of water, ethanol, and acetone. It is understood that the solvent may include any one of water, ethanol and acetone, or a mixture of several of water, ethanol and acetone.
In some embodiments, the process conditions for spray granulation include: the diameter of the nozzle is 0.1 mm-3 mm, the temperature of the air inlet is 50-250 ℃, the temperature of the air outlet is 40-200 ℃, the rotating speed of the peristaltic pump is 20 r/min-80 r/min, and the rotating speed of the fan is 20 r/min-80 r/min. It will be appreciated that the nozzle diameter may be anywhere between 0.1mm and 3mm, and may for example be 0.1mm, 0.2mm, 0.5mm, 0.8mm, 1mm, 1.2mm, 1.4mm, 1.6mm, 1.8mm, 2mm, 2.2mm, 2.4mm, 2.6mm, 2.8mm or 3mm; the temperature of the air inlet can be 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 110 ℃, 120 ℃, 150 ℃, 180 ℃, 200 ℃, 220 ℃ or 250 ℃, or other values between 50 ℃ and 250 ℃; the air outlet temperature can be 40 deg.C, 50 deg.C, 60 deg.C, 70 deg.C, 80 deg.C, 90 deg.C, 100 deg.C, 110 deg.C, 120 deg.C, 130 deg.C, 140 deg.C, 150 deg.C, 170 deg.C, 190 deg.C or 200 deg.C, etc.; the rotating speed of the peristaltic pump can be 20r/min, 25r/min, 30r/min, 35r/min, 40r/min, 45r/min, 50r/min, 60r/min, 70r/min or 80r/min, etc., the rotating speed of the fan can be 20r/min, 25r/min, 30r/min, 35r/min, 40r/min, 45r/min, 50r/min, 55r/min, 60r/min, 65r/min, 70r/min or 80r/min, etc., and can also be other values between 20r/min and 80r/min.
In another aspect of the application, a chromium aluminum carbide ceramic is provided, which is prepared by the preparation method.
In some embodiments, the chromium aluminum carbide ceramic has a D10 of 4 to 8 μm, a D50 of 20 to 28 μm, a D90 of 35 to 42 μm, and a specific surface area of 400m 2 /kg～550m 2 Kg, bulk density of 0.957g/cm 3 ～1.527g/cm 3 。
It should be noted that "D10" means a particle diameter having a cumulative particle size distribution of 10%, that is, the volume content of particles smaller than this particle diameter is 10% of the total particles; "D50" refers to a cumulative particle distribution of 50% of the particle size, i.e., the median or average particle size, i.e., 50% of the particles are above this value and 50% are below this value; "D90" refers to a particle size having a cumulative particle distribution of 90%, i.e., the volume fraction of particles smaller than this particle size is 90% of the total particles. It is understood that D10 of the chromium aluminum carbide ceramic may be any value between 4 μm and 8 μm, and may be, for example, 4 μm, 4.5 μm, 5 μm, 5.5 μm, 6 μm, 6.5 μm, 7 μm, 7.5 μm, 8 μm, or the like; the D50 of the chromium aluminum carbide ceramic may be, for example, 20 μm, 21 μm, 22 μm, 23 μm, 24 μm, 25 μm, 26 μm, 27 μm, or 28 μm; d90 of the chromium aluminum carbide ceramic includes but is not limited to may be 35 μm, 36 μm, 37 μm, 38 μm, 39 μm, 40 μm, 41 μm, 42 μm, or the like; the specific surface area of the chromium aluminum carbide ceramic includes, but is not limited to, may be 400m 2 /kg、410m 2 /kg、420m 2 /kg、430m 2 /kg、440m 2 /kg、450m 2 /kg、460m 2 /kg、470m 2 /kg、480m 2 /kg、490m 2 /kg、500m 2 /kg、520m 2 /kg、540m 2 /kg or 550m 2 Per kg; the apparent density of the chromium aluminum carbide ceramic includes, but is not limited to, can be 0.957g/cm 3 、0.968g/cm 3 、0.975g/cm 3 、0.983g/cm 3 、0.997g/cm 3 、1.057g/cm 3 、1.123g/cm 3 、1.246g/cm 3 、1.375g/cm 3 、1.422g/cm 3 Or 1.527g/cm 3 The apparent density of the chromium aluminum carbide ceramic may also be 0.957g/cm 3 ～1.527g/cm 3 Other values in between.
In a further aspect of the present application, there is provided a chromium aluminum carbide ceramic prepared by the above preparation method or use of the above chromium aluminum carbide ceramic in a thermal spraying process.
In some embodiments, the chromium aluminum carbide ceramic is formed into a high temperature protective coating, a high temperature coating transition layer, or a corrosion resistant coating using a thermal spray process.
It should be noted that the chromium-aluminum carbide ceramic is used as a raw material, and can be made into a high-temperature protective coating, a high-temperature coating transition layer or an anti-corrosion coating by adopting a thermal spraying process. Alternatively, thermal spray process techniques include, but are not limited to, plasma Spray (PS), atmospheric Plasma Spray (APS), low Pressure Plasma Spray (LPPS), ultra low pressure plasma spray (VLPPS), plasma spray-physical vapor deposition (PS-PVD), suspension Plasma Spray (SPS), high velocity oxy-fuel (HVOF, HVAF), and the like.
As the parameter measurement in the present application, optionally, the following apparatus and method are employed for measurement:
test methods for D10, D50 and D90: the measurement was carried out by a laser method using a BT-9300ST type laser particle size analyzer.
The loose packed density test method comprises the following steps: the measurement is carried out by a funnel method or a vibration funnel method.
Specific surface area test method: the determination is carried out by adopting a Congta Autosorb-iQ-3 type BET specific surface full-automatic physical adsorption analyzer through a gas adsorption method.
The present application will be described in further detail with reference to specific examples.
Example 1
The mixed grinding ball of the embodiment is formed by grinding three zirconia grinding balls with the diameters of 1mm, 5mm and 8mm according to the weight ratio of 1:1: 1.
The chromium aluminum carbide ceramic powder was prepared as follows:
s1, carrying out ball-milling pretreatment on chromium powder
Mixing a mixed grinding ball, chromium powder (Cr-325 meshes, and the purity is not less than 99.9%) and ball milling medium ethanol according to the weight ratio of 2:1:1.1 adding the mixture into a ball milling tank, ball milling the mixture for 8 hours at the rotating speed of 400r/min, and then drying the chromium powder suspension obtained after ball milling in a vacuum oven for 2 hours at the temperature of 80 ℃ to obtain refined chromium powder, wherein the average grain diameter D50 of the chromium powder is 10 microns;
s2, mixing the chromium powder and the aluminum powder (Al, with the particle size of-200 meshes and the purity of 99.9% or more) obtained in the step S1 and the graphite powder (C, with the particle size of-325 meshes and the purity of 99.9% or more) according to a molar ratio of 2:1.1:1, mixing to form a mixed material, and mixing a mixed grinding ball, the mixed material and ball-milling medium ethanol according to a weight ratio of 3:1:1.5 adding the mixture into a ball milling tank, ball milling the mixture for 4 hours at the rotating speed of 400r/min, and drying the mixed material suspension obtained after ball milling for 3 hours in a vacuum oven at the temperature of 60 ℃ to obtain uniformly mixed powder with the average particle size D50 of 14 microns;
s3, mixing the powder obtained in the step S2 under the vacuum degree of 4 multiplied by 10 -3 In a Pa vacuum furnace, the temperature is raised from room temperature to 1100 ℃ at the temperature-raising rate of 7 ℃/min for sintering for 8h to obtain a precursor (Cr) 2 AlC bulk material);
s4, crushing the precursor obtained in the step S3, and performing high-energy ball milling on the crushed precursor, deionized water, a binder polyvinyl alcohol (PVA) and a dispersant ammonium polyacrylate to obtain slurry, wherein the slurry comprises the following substances in percentage by weight: 15% of precursor, 1% of binder, 2% of dispersant and 82% of deionized water;
s5, after the slurry obtained in the step S4 is adjusted to be alkalescent by ammonia water, preparing chromium aluminum carbide ceramic powder by adopting a centrifugal spray granulation process, wherein the spray granulation process conditions comprise: the air inlet temperature is 150 ℃, the air outlet temperature is 100 ℃, the rotating speed of the peristaltic pump is 50r/min, and the rotating speed of the fan is 60r/min;
s6, subsequently sieving the chromium aluminum carbide ceramic powder to obtain the chromium aluminum carbide ceramic powder suitable for thermal spraying, wherein the chromium aluminum carbide ceramic powder has the D10 of 5 microns, the D50 of 24 microns, the D90 of 37 microns and the apparent density of 1.049g/cm 3 Specific surface area of 495m 2 /kg；
S7, spraying the chromium-aluminum carbide ceramic powder prepared in the step S6 on a substrate by using a supersonic flame spraying technology to form a chromium-aluminum carbide coating, wherein the process conditions of the supersonic flame spraying technology comprise: argon is used as powder feeding protective gas, the working distance is 220mm, and the propane flow is 30 L.min -1 The oxygen flow is 40 L.min -1 The powder feeding amount is 20 g/min -1 。
Example 2
The mixed grinding ball of the embodiment is formed by grinding three zirconia grinding balls with the diameters of 1mm, 5mm and 8mm according to the weight ratio of 1:1.1: 1.1.
The chromium aluminum carbide ceramic powder was prepared as follows:
s1, carrying out ball-milling pretreatment on chromium powder
Mixing the mixed grinding ball and chromium powder (Cr, -325 meshes, purity ≧ 99.9%) according to a weight ratio of 5:1, adding the mixture into a ball milling tank, and carrying out ball milling for 10 hours at the rotating speed of 350r/min under the argon protective atmosphere to obtain refined chromium powder, wherein the average particle size D50 of the chromium powder is 13 microns;
s2, mixing the chromium powder and the aluminum powder (Al, with the particle size of-200 meshes and the purity of 99.9% or more) obtained in the step S1 and the graphite powder (C, with the particle size of-325 meshes and the purity of 99.9% or more) according to a molar ratio of 2:1.1:1, mixing to form a mixed material, and mixing the mixed grinding ball and the mixed material according to the weight ratio of 5:1, adding the mixture into a ball milling tank, and ball milling the mixture for 6 hours at the rotating speed of 350r/min to obtain uniformly mixed powder, wherein the average particle size D50 of the uniformly mixed powder is 16 microns;
s3, mixing the powder obtained in the step S2 under the vacuum degree of 3.7 multiplied by 10 -3 In a Pa vacuum furnace, the temperature is raised from room temperature to 1100 ℃ at the temperature-raising rate of 7 ℃/min for sintering for 8h to obtain a precursor (Cr) 2 AlC bulk);
s4, crushing the precursor obtained in the step S3, and performing high-energy ball milling on the crushed precursor, deionized water, a binder hydroxymethyl cellulose (CMC) and a dispersant ammonium polyacrylate to obtain slurry, wherein the slurry comprises the following substances in percentage by weight: 15% of precursor, 2% of binder, 1% of dispersant and 82% of deionized water;
s5, preparing the slurry obtained in the step S4 into alkalescence by ammonia water, and then preparing chromium-aluminum carbide ceramic powder by adopting a centrifugal spray granulation process, wherein the spray granulation process conditions comprise: the air inlet temperature is 150 ℃, the air outlet temperature is 100 ℃, the rotating speed of the peristaltic pump is 50r/min, and the rotating speed of the fan is 60r/min;
s6, subsequently sieving the chromium aluminum carbide ceramic powder to obtain the chromium aluminum carbide ceramic powder suitable for thermal spraying, wherein the D10 is 7 mu m, the D50 is 28 mu m, the D90 is 40 mu m, and the apparent density is 1.137g/cm 3 Specific surface area of 411m 2 /kg；
S7, spraying the chromium-aluminum carbide ceramic powder prepared in the step S6 on a substrate by using a supersonic flame spraying technology to form a chromium-aluminum carbide coating, wherein the process conditions of the supersonic flame spraying technology comprise: argon is used as powder feeding protective gas, the working distance is 220mm, the propane flow is 30 L.min -1 The oxygen flow is 40 L.min -1 The powder feeding amount is 20 g/min -1 。
Example 3
This example is specifically the same as example 1, except that: in step S2, the chromium powder and aluminum powder (Al-200 mesh, purity ≧ 99.9%) obtained in step S1, and graphite powder (C-325 mesh, purity ≧ 99.9%) are mixed in a molar ratio of 2:1:1, mixing to form a mixed material.
The chromium aluminum carbide ceramic powder prepared in this example had a D10 of 6 μm, a D50 of 25 μm, a D90 of 41 μm, and a bulk density of 0.979g/cm 3 Specific surface area of 478m 2 /kg。
Example 4
This example is specifically the same as example 1, except that: in step S2, the chromium powder and aluminum powder (Al-200 mesh, purity ≧ 99.9%) obtained in step S1, and graphite powder (C-325 mesh, purity ≧ 99.9%) are mixed in a molar ratio of 2:1.05:1, mixing to form a mixed material.
The chromium aluminum carbide ceramic powder prepared in this example had a D10 of 6 μm,d50 is 22 μm, D90 is 35 μm, and the loose packed density is 1.017g/cm 3 The specific surface area is 534m 2 /kg。
Example 5
This example is specifically the same as example 2, except that: in step S2, the chromium powder and the aluminum powder (Al-200 mesh, purity ≧ 99.9%), the graphite powder (C-325 mesh, purity ≧ 99.9%) obtained in step S1 are mixed in a molar ratio of 2:1:1, mixing to form a mixed material.
The chromium aluminum carbide ceramic powder prepared in this example had a D10 of 7 μm, a D50 of 28 μm, a D90 of 42 μm, and a bulk density of 1.344g/cm 3 Specific surface area of 400m 2 /kg。
Example 6
This embodiment is specifically the same as embodiment 2, except that: in step S2, the chromium powder and aluminum powder (Al-200 mesh, purity ≧ 99.9%) obtained in step S1, and graphite powder (C-325 mesh, purity ≧ 99.9%) are mixed in a molar ratio of 2:1.05:1 mixing to form a mixed material.
The chromium aluminum carbide ceramic powder prepared in this example had a D10 of 8 μm, a D50 of 26 μm, a D90 of 41 μm, and a bulk density of 1.220g/cm 3 Specific surface area of 424m 2 /kg。
Test results
Fig. 2 is an X-ray diffraction pattern of the chromium aluminum carbide ceramic powder prepared in example 1, and it can be seen from fig. 2 that the product prepared in example 1 is the chromium aluminum carbide ceramic powder, and the prepared chromium aluminum carbide ceramic powder has high purity and no obvious impurities.
Fig. 3 is an SEM image of the chromium aluminum carbide ceramic powder prepared in example 1, fig. 4 is a cross-sectional SEM image of the chromium aluminum carbide ceramic powder prepared in example 1, and fig. 3 to 4 can illustrate that the chromium aluminum carbide ceramic powder prepared in example 1 has better sphericity and thus better fluidity, which is advantageous for applying it to a thermal spraying process.
Fig. 5 is a cross-sectional SEM image of the chromium-aluminum carbide coating prepared in example 2, and as can be seen from fig. 5, the thickness of the chromium-aluminum carbide coating in example 2 is 120 μm to 150 μm, and by combining fig. 5 and performing image statistics, the porosity of the chromium-aluminum carbide coating in example 2 is 5% and the density is 95%, which indicates that the chromium-aluminum carbide coating prepared in example 2 is dense, has good bonding with the substrate, can perform a sufficient thermal shock protection function, and improves the thermal shock resistance and the high temperature corrosion resistance.
The chromium aluminum carbide ceramic powders prepared in examples 2 to 6 were also subjected to SEM and cross-sectional SEM tests, and the results obtained were similar to those of the test in example 1. Similarly, cross-sectional SEM tests were performed on the chromium aluminum carbide coatings prepared in examples 1 and 3-6, and the results were similar to those of example 2. Therefore, the preparation method can improve the sphericity, the fluidity, the purity, the thermal shock resistance and the high-temperature corrosion resistance of the chromium-aluminum carbide ceramic powder, further reduce the preparation difficulty of the chromium-aluminum carbide coating and improve the preparation efficiency and the quality of the coating.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent should be subject to the appended claims, and the description and drawings can be used to explain the contents of the claims.
Claims (10)
1. The preparation method of the chromium aluminum carbide ceramic is characterized by comprising the following steps:
s1, carrying out ball-milling pretreatment on chromium powder;
s2, aluminum powder, carbon powder and chromium powder obtained by the pre-ball milling treatment are mixed according to the molar ratio (1-1.1): 1:2, ball milling after mixing to obtain mixed powder;
s3, sintering the mixed powder under a protective atmosphere or vacuum condition to obtain a precursor;
s4, crushing the precursor, and ball-milling the crushed precursor, the solvent, the binder and the dispersant to obtain slurry;
and S5, adjusting the pH value of the slurry to be alkaline, and then performing spray granulation to obtain the chromium aluminum carbide ceramic.
2. The preparation method according to claim 1, wherein the slurry comprises, in mass percent: 10 to 20 percent of precursor, 1 to 2 percent of binder, 0.5 to 2 percent of dispersant and 78.5 to 86 percent of solvent.
3. The preparation method according to claim 1, wherein the particle size of the chromium powder is 325 to 800 meshes, the particle size of the aluminum powder is 200 to 400 meshes, and the particle size of the carbon powder is 325 to 800 meshes.
4. The preparation method according to claim 1, wherein the average particle diameter D50 of the chromium powder obtained by the pre-ball milling is 10 to 15 μm, and the average particle diameter D50 of the mixed powder is 12 to 16 μm.
5. The production method according to any one of claims 1 to 4, characterized by comprising at least one of the following features (1) to (6):
(1) The protective atmosphere comprises one or more of inert gas and nitrogen;
(2) The protective atmosphere comprises one or more of inert gas and nitrogen, and the inert gas comprises one or more of helium, neon, argon, krypton and xenon;
(3) The degree of vacuum of the sintering is 1 x 10 -3 Pa～5×10 -3 Pa；
(4) The temperature rise rate of the sintering is 5-10 ℃/min;
(5) The sintering temperature is 1050-1150 ℃;
(6) The sintering time is 6-10 h.
6. The production method according to any one of claims 1 to 4, characterized by comprising at least one of the following features (1) to (3):
(1) The binder comprises one or more of polyvinyl alcohol, polystyrene and hydroxymethyl cellulose;
(2) The dispersant comprises ammonium polyacrylate;
(3) The solvent comprises one or more of water, ethanol and acetone.
7. The method according to any one of claims 1 to 4, wherein the process conditions of the spray granulation include: the diameter of the nozzle is 0.1 mm-3 mm, the air inlet temperature is 50-250 ℃, the air outlet temperature is 40-200 ℃, the rotation speed of the peristaltic pump is 20 r/min-80 r/min, and the rotation speed of the fan is 20 r/min-80 r/min.
8. A chromium aluminum carbide ceramic produced by the production method according to any one of claims 1 to 7.
9. The chromium aluminum carbide ceramic according to claim 8, wherein the chromium aluminum carbide ceramic has a D10 of 4 to 8 μm, a D50 of 20 to 28 μm, a D90 of 35 to 42 μm, and a specific surface area of 400m 2 /kg～550m 2 Kg, bulk density of 0.957g/cm 3 ～1.527g/cm 3 。
10. Use of a chromium aluminium carbide ceramic produced by a method according to any one of claims 1 to 7 or a chromium aluminium carbide ceramic according to any one of claims 8 to 9 in a thermal spray process.
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