CN113511912A - Wear-resistant corrosion-resistant carbide ceramic coating and preparation method thereof - Google Patents
Wear-resistant corrosion-resistant carbide ceramic coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a wear-resistant and corrosion-resistant carbide ceramic coating and a preparation method thereof, belonging to the technical field of coatings. The preparation method adopts a dipping and pulling method to dip the matrix in a dipping solution to obtain the dipped matrix; and sequentially carrying out cross-linking treatment and pyrolysis treatment on the impregnated matrix to prepare the wear-resistant corrosion-resistant carbide ceramic coating on the matrix. The wear-resistant corrosion-resistant carbide ceramic coating prepared by the preparation method solves the problems of complex preparation and high cost of the existing SiC ceramic coating and large contractibility of the existing SiC ceramic coating prepared by the existing dipping method process, and ensures good bonding property, compactness, continuity and effective corrosion resistance of the wear-resistant corrosion-resistant carbide ceramic coating and a matrix.
Description
Technical Field
The invention belongs to the technical field of coatings, and relates to a wear-resistant corrosion-resistant carbide ceramic coating and a preparation method thereof.
Background
Although the annual output of steel, which is one of the economic shoring industries in China, is in the forefront of the world, the annual waste amount is also remarkable. For example, metal components that are exposed to highly reactive or corrosive environments for extended periods of time are highly susceptible to corrosion and damage due to oxidation, however, the cost of maintaining and replacing these materials is high, thereby resulting in a significant waste of resources. The coating can play an effective protection role on the oxidation corrosion of steel, so that the coating with corrosion resistance can be used as an effective method for solving the problem. The carbide has the characteristics of high stability, high hardness, excellent wear resistance and the like, wherein the silicon carbide has the excellent characteristics of high-temperature stability, high hardness, oxidation resistance, corrosion resistance, high chemical inertness and the like, so that the silicon carbide coating can be applied to the protection of steel materials, and the service life of the steel materials is prolonged.
The common preparation method of the carbide coating comprises the following steps: chemical vapor deposition, plasma spraying, vacuum arc deposition, etc., but these methods are complicated in operation process and high in production cost, and are not suitable for industrial mass production. The dipping and pulling method has low production cost and wide requirements on the size and shape range of the workpiece due to convenient operation technology, is suitable for industrial batch production, and is usually combined with a precursor cracking method to prepare the SiC coating in the current scientific research work. But the precursor cracking method can generate larger volume shrinkage during cracking, thereby influencing the compactness, continuity and binding property with a substrate of the coating; meanwhile, in order to meet the requirements of actual use on performance, a coating with good protection effect needs to be prepared, namely the SiC coating needs to have the characteristics of high stability, compactness and continuity. Therefore, how to effectively reduce the large volume shrinkage of the SiC coating in the cracking process becomes a key problem to be solved in the preparation process of the well developed SiC coating at present.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a wear-resistant corrosion-resistant carbide ceramic coating and a preparation method thereof, which solve the problems of complex preparation method of a SiC coating, high cost and large shrinkage of the SiC coating prepared by the existing dipping method process, and further avoid the problem of poor bonding between the coating prepared by the existing dipping method process and a substrate.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a preparation method of a wear-resistant and corrosion-resistant carbide ceramic coating, which comprises the steps of adopting a dipping and pulling method to dip a substrate in a dipping solution to obtain a dipped substrate; sequentially carrying out cross-linking treatment and pyrolysis treatment on the impregnated matrix to prepare a wear-resistant corrosion-resistant carbide ceramic coating on the matrix; the impregnation liquid comprises a SiC precursor, a SiC precursor solvent, an inert filler, a glass filler, a fiber filler and a dispersing agent.
Preferably, the SiC precursor is polycarbosilane; the SiC precursor solvent is xylene, toluene, tetrahydrofuran or chloroform.
Preferably, the inert filler is SiC powder or SiO2Powder; the glass filler is commercial ST880 powder; the fibrous filler is a carbide fiber or an oxide fiber.
Further preferably, the fibrous filler is SiC fiber, Al2O3Fibres or ZrO2A fiber.
Preferably, the impregnation liquid is prepared according to the following formula:
a) the proportion of the SiC precursor to the SiC precursor solvent is as follows:
wherein: mpMass/g, V of SiC precursors-volume/mL of SiC precursor solvent;
b) the proportion of the SiC precursor to the inert filler, the glass filler and the fiber filler is as follows:
wherein: mpMass/g, M of SiC precursorInertia deviceMass/g, M of inert fillergMass/g, M of glass fillerf-mass of fibrous filler/g;
c) the amount of dispersant is calculated as follows:
Md＝(Minertia device+Mg+Mf)×0.02～0.04；
Wherein: mInertia deviceMass/g, M of inert fillergMass/g, M of glass fillerdMass of dispersant/g, Mf-mass of fibrous filler/g.
Preferably, the preparation process of the impregnation liquid comprises the following steps: firstly, dissolving a SiC precursor in a SiC precursor solvent to obtain a precursor solution, then uniformly dispersing a dispersing agent in the obtained precursor solution to obtain a solution A, and finally uniformly dispersing a fiber filler, an inert filler and a glass filler in the obtained solution A to obtain an impregnation solution.
Preferably, the operation of the dip-draw method comprises: dipping the substrate at a descending speed of 800-1500 μm/s and a pulling speed of 800-1500 μm/s, wherein the substrate is kept in the dipping solution for 2-5 min, and the cycle is 1-3 times.
Preferably, the process parameters of the cross-linking treatment include: heating to 180-200 ℃ at a heating rate of 1-2 ℃/min, preserving heat for 2-3 h, and cooling to room temperature at a cooling rate of 1-2 ℃/min.
Preferably, the process parameters of the pyrolysis treatment include: heating to 350-450 ℃ at a heating rate of 3-4 ℃/min, heating to 850-950 ℃ at a heating rate of 2-3 ℃/min, preserving heat for 1-2 h, cooling to 350-450 ℃ at a cooling rate of 2-3 ℃/min, and cooling to room temperature at a cooling rate of 3-4 ℃/min.
The invention discloses a wear-resistant corrosion-resistant carbide ceramic coating prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the wear-resistant corrosion-resistant carbide ceramic coating, the preparation process of the SiC coating is simplified by adopting the dip-coating method, the cost for preparing the SiC coating is effectively reduced, the requirements of the dip-coating method on the shape and size ranges of the workpiece are low, and the application range of the SiC coating is favorably expanded. By adding a certain amount of inert filler and fiber filler with a certain size range into the SiC precursor, the SiC precursor can be effectively inhibited from generating larger volume shrinkage during cracking. By adding the glass filler with certain initial melting temperature into the system, the glass filler which is gradually melted in the cracking process further fills cracks and air holes generated in the cracking process of the coating, so that the compactness of the coating is further increased, the corrosion resistance of the coating is effectively improved, and the problems of large shrinkage of the SiC coating prepared by the existing dipping method process and poor combination between the coating prepared by the existing dipping method process and the matrix are solved. Therefore, the preparation method of the wear-resistant and corrosion-resistant carbide ceramic coating has the advantages that the compactness of the coating prepared by the method is good, the corrosion resistance of the SiC coating is effectively improved, the operation process is convenient and fast, the preparation method is suitable for substrates with various shapes, the economic benefit is high, and the preparation method is suitable for industrial batch production.
Further, Polycarbosilane (PCS) is adopted as a precursor of the SiC coating, so that the problem that SiC in the coating is difficult to distribute uniformly is solved.
The invention also discloses a wear-resistant corrosion-resistant carbide ceramic coating prepared by the preparation method, and the wear-resistant corrosion-resistant carbide ceramic coating can effectively inhibit the SiC precursor from generating larger volume shrinkage during cracking due to the addition of a certain amount of inert filler, fiber filler and glass filler with a certain size range into the SiC precursor, and further fills cracks and air holes generated during the cracking of the coating by the gradually-melted glass filler in the cracking process, so that the compactness of the coating is further increased, the corrosion resistance of the coating is effectively improved, the problems of high complexity and cost of the preparation method of the SiC coating and large shrinkage of the SiC coating prepared by the existing dipping method process are solved, and the problem of poor combination between the coating prepared by the existing dipping method process and a substrate is further avoided.
Drawings
FIG. 1 is a surface topography of a wear and corrosion resistant carbide ceramic coating prepared in example 1 of the present invention.
FIG. 2 is a potentiodynamic polarization curve comparing a wear and corrosion resistant carbide ceramic coating prepared in example 1 of the present invention with a steel substrate.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention discloses a preparation method of a wear-resistant and corrosion-resistant carbide ceramic coating, which specifically comprises the following steps.
Step 1: pretreatment of substrates
The surface oxide skin of the substrate is firstly polished by abrasive paper, and then the substrate is sequentially polished by thinner abrasive paper until the surface of the substrate is smooth and has consistent roughness. And (3) putting the polished substrate into absolute ethyl alcohol for ultrasonic treatment for 10-15 min, and removing the residual abrasive particles and other pollution stains on the surface of the substrate. Drying the substrate subjected to ultrasonic treatment in an oven at 60 ℃ for 10-30 min so as to completely volatilize the absolute ethyl alcohol on the surface of the substrate and ensure that the surface of the substrate is clean and pollution-free; and finishing the pretreatment of the substrate according to the requirements to obtain a clean substrate.
Step 2: preparation of impregnation liquid and impregnation of matrix
Weighing a certain amount of SiC precursor according to the formula (1) and dissolving the SiC precursor in a SiC precursor solvent, stirring for 10-20 min until the SiC precursor is fully dissolved to obtain a precursor solution, then weighing a certain amount of dispersant (any substance with a dispersing effect in an organic solvent can be used as the dispersant in the system) according to the formula (5), adding the dispersant into the obtained precursor solution, stirring for 3-10 min to uniformly disperse the dispersant in the obtained precursor solution, wherein the obtained solution is called solution A, then weighing a certain amount of inert filler, fiber filler and glass filler according to the formula (2), the formula (3) and the formula (4), adding the inert filler, the fiber filler and the glass filler into the solution A, stirring for 4-6 h to fully disperse the fillers in the solution A, wherein the obtained solution is called solution B, and the solution B is an impregnation solution, so that the preparation of the impregnation solution is finished. And (2) suspending the base body pretreated according to the requirement of the step (1) on an impregnation drawing machine, dipping at a descending speed of 800-1500 mu m/s and a drawing speed of 800-1500 mu m/s, standing the base body in a dipping solution for 2-5 min, and circulating for 1-3 times to finish dipping of the base body to obtain the dipped base body.
The ratio of the SiC precursor to the SiC precursor solvent is shown in formula (1):
wherein: mpMass/g, V of SiC precursors-volume/mL of SiC precursor solvent;
the proportion of the SiC precursor to the inert filler, the fiber filler and the glass filler is shown in formula (2), formula (3) and formula (4):
wherein: mpMass/g, M of SiC precursorInertia deviceMass/g, M of inert fillergMass/g, M of glass fillerf-mass of fibrous filler/g;
the amount of dispersant is calculated according to equation (5):
Md＝(Minertia device+Mg+Mf)×0.02～0.04 (5)
Wherein: mInertia deviceMass/g, M of inert fillergMass/g, M of glass fillerdMass of dispersant/g, Mf-mass of fibrous filler/g;
the SiC precursor is Polycarbosilane (PCS), the SiC precursor solvent is dimethylbenzene, methylbenzene, tetrahydrofuran or chloroform, and the inert filler is SiC powder or SiO2Powder (average particle size of 0.1-0.7 μm), wherein the glass filler is commercial ST880 powder (initial melting temperature of 690 ℃ and average particle size of 8 μm), and the fiber filler is carbide fiber such as SiC fiber or Al2O3Fiber, ZrO2Oxide fiber (fiber) such as fiberDiameter of 5-7 μm and average fiber length of 20-25 μm).
And step 3: the cross-linking and pyrolysis of the coating can prepare a wear-resistant and corrosion-resistant carbide ceramic coating
And (3) placing the substrate soaked according to the requirements in a blast drying oven, heating to 180-200 ℃ at a heating rate of 1-2 ℃/min in air atmosphere, preserving the heat for 2-3 h, cooling to room temperature (15-35 ℃) at a cooling rate of 1-2 ℃/min, and finishing the crosslinking process of the coating to obtain the substrate with the crosslinked surface coating. And (2) placing the substrate with the surface coating crosslinked in a vacuum tube furnace, changing the air in the furnace tube into argon, heating to 350-450 ℃ at the heating rate of 3-4 ℃/min, then heating to 850-950 ℃ at the heating rate of 2-3 ℃/min, preserving the heat for 1-2 h, cooling to 350-450 ℃ at the cooling rate of 2-3 ℃/min, and then cooling to room temperature at the cooling rate of 3-4 ℃/min, thus completing the pyrolysis process of the coating, and forming a compact wear-resistant corrosion-resistant carbide ceramic coating on the surface of the substrate.
In the specific embodiment of the present invention, the dispersant may be selected from a basf dispersant, model number Efka FA 4663AN, or castor oil phosphate.
In particular, in the embodiment of the invention, the wear-resistant and corrosion-resistant carbide ceramic coating has high continuity, good compactness and good bonding property with the matrix, and improves the corrosion resistance of the matrix. The thickness is 15 to 45 μm.
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
A preparation method of a wear-resistant corrosion-resistant carbide ceramic coating specifically comprises the following steps:
step 1: pretreatment of substrates
The Q235 steel is firstly polished to remove oxide skin on the surface by using No.320 abrasive paper, and then sequentially polished to be smooth and consistent in roughness on the surface of the metal substrate by using No.600 abrasive paper and No.800 abrasive paper respectively. And (3) putting the polished metal matrix into absolute ethyl alcohol for ultrasonic treatment for 10min, and removing the residual abrasive particles and other pollution stains on the surface of the metal matrix. And (3) drying the metal matrix subjected to ultrasonic treatment in a drying oven at 60 ℃ for 15min so as to completely volatilize the absolute ethyl alcohol on the surface of the metal matrix and ensure that the metal surface is clean and pollution-free, and finishing pretreatment of the matrix according to the requirements to obtain a clean matrix.
Step 2: preparation of impregnation liquid and impregnation of metal matrix
Push button
Weighing 5.5g PCS to dissolve in 11mL dimethylbenzene, sealing the opening with a preservative film because the dimethylbenzene is volatile, stirring for 10min to fully dissolve PCS in the dimethylbenzene to obtain a PCS solution, and then adding Md＝(MInertia device+Mg+Mf) 0.03 weighing 0.15g of Pasteur dispersant (model Efka FA 4663AN), adding the dispersant to the PCS solution obtained above, stirring for 5min to disperse the dispersant uniformly in the solution, the solution obtained at this time being called solution A, and then
2.75g of SiC powder, 0.33g of SiC fibers, and 1.925g of ST880 were weighed out. Adding 2.75g of SiC powder into the solution A, stirring for 3min, then respectively adding 1.925g of ST880 and 0.33g of SiC fiber, stirring for 5.5h, fully dispersing the three fillers into the solution A to form a solution B, wherein the solution B is the prepared impregnation solution, suspending the metal matrix pretreated according to the requirements on an impregnation drawing machine, impregnating at a descending speed of 800 mu m/s and a drawing speed of 800 mu m/s, standing the matrix in the impregnation solution for 3min, and circulating for 1 time.
And step 3: the cross-linking and pyrolysis of the coating can prepare a wear-resistant and corrosion-resistant carbide ceramic coating
And (3) placing the substrate soaked according to the requirements in a blast drying oven, heating to 190 ℃ at the heating rate of 1 ℃/min in the air atmosphere, preserving the heat for 2h, and cooling to room temperature at the cooling rate of 1 ℃/min, thus completing the crosslinking process of the coating and obtaining the metal substrate with the crosslinked surface coating. And (3) placing the substrate with the crosslinked surface coating in a vacuum tube furnace, changing the air in the furnace tube into argon, heating to 400 ℃ at the heating rate of 3 ℃/min, then heating to 900 ℃ at the heating rate of 2 ℃, preserving the heat for 1h, cooling to 400 ℃ at the cooling rate of 2 ℃/min, and then cooling to room temperature at the cooling rate of 3 ℃/min, thus completing the pyrolysis process of PCS, forming a compact wear-resistant corrosion-resistant SiC ceramic coating on the surface of the metal substrate, wherein the thickness of the prepared coating is about 15 mu m.
An electron microscope scanning image of the wear-resistant and corrosion-resistant SiC ceramic coating prepared in the example is shown in FIG. 1. The corrosion resistance potentiodynamic polarization curve is shown in FIG. 2. (the testing equipment of the zeta potential polarization curve is American Aromatk group PARSTAT 4000A electrochemical workstation), the method can be obtained from the graph 1, and under the magnification of 50 times, the prepared SiC coating has no large cracks on the surface, high continuity of the coating surface and good compactness. Fig. 2 is a potentiodynamic polarization curve of the SiC ceramic coating and the Q235 steel substrate without the coating in example 1 tested in a 3.5 wt% NaCl solution, and it can be seen from the graph that the Q235 steel substrate with the SiC ceramic coating has a lower self-corrosion current density than the Q235 steel substrate without the SiC coating, so that under the test conditions, the Q235 steel substrate protected by the SiC ceramic coating has a lower corrosion rate than the Q235 steel substrate without the SiC coating, so that the SiC ceramic coating prepared in example 1 can effectively protect the steel substrate, and the corrosion resistance of the steel is increased.
Example 2
A preparation method of a wear-resistant corrosion-resistant carbide ceramic coating specifically comprises the following steps:
step 1: pretreatment of metal substrates
The Q235 steel is firstly polished to remove oxide skin on the surface by using No.320 abrasive paper, and then sequentially polished to be smooth and consistent in roughness on the surface of the metal substrate by using No.600 abrasive paper and No.800 abrasive paper respectively. And (3) putting the polished metal matrix into absolute ethyl alcohol for ultrasonic treatment for 15min, and removing the residual abrasive particles and other pollution stains on the surface of the metal matrix. And (3) drying the metal matrix subjected to ultrasonic treatment in a drying oven at 60 ℃ for 30min so as to completely volatilize the absolute ethyl alcohol on the surface of the metal matrix and ensure that the metal surface is clean and pollution-free, and finishing pretreatment of the matrix according to the requirements to obtain a clean matrix.
Step 2: preparation of impregnation liquid and impregnation of metal matrix
Push button
Weighing 6.6g of PCS to dissolve in 11mL of dimethylbenzene, sealing the opening of thed＝(MInertia device+Mg+Mf) 0.02 weight of 0.139g of Pasteur dispersant (model Efka FA 4663AN), add the dispersant to the PCS solution obtained above, stir for 10min to disperse the dispersant uniformly in the solution, the solution obtained at this time is called solution A, then add
3.63g of SiO were weighed in each case2Powder, 2.97g of ST880 and 0.33g of SiC fiber. To the solution A was added 3.63g of SiO2Stirring the powder for 3min, then respectively adding 2.97g of ST880 and 0.33g of SiC fiber, stirring for 6h, fully dispersing the three fillers in the solution A to form a solution B, wherein the solution B is the prepared impregnation liquid, suspending the metal matrix pretreated according to the requirements on an impregnation pulling machine, impregnating at a descending speed of 1500 mu m/s and a pulling speed of 1500 mu m/s, standing the matrix in the impregnation liquid for 5min, and circulating for 2 times.
And step 3: the cross-linking and pyrolysis of the coating can prepare a wear-resistant and corrosion-resistant carbide ceramic coating
And (3) placing the substrate soaked according to the requirements in a blast drying oven, heating to 200 ℃ at a heating rate of 2 ℃/min in the air atmosphere, preserving the heat for 2h, and cooling to room temperature at a cooling rate of 2 ℃/min, thus completing the crosslinking process of the coating and obtaining the metal substrate with the surface coating crosslinked. And (3) placing the substrate with the crosslinked surface coating in a vacuum tube furnace, changing the air in the furnace tube into argon, heating to 450 ℃ at the heating rate of 4 ℃/min, then heating to 950 ℃ at the heating rate of 3 ℃/min, preserving the heat for 1h, cooling to 450 ℃ at the cooling rate of 3 ℃/min, and then cooling to room temperature at the cooling rate of 4 ℃/min, thus completing the pyrolysis process of PCS (polycarbonate-coated ceramic), forming a compact wear-resistant corrosion-resistant SiC ceramic coating on the surface of the metal substrate, wherein the thickness of the prepared coating is about 30 mu m.
Example 3
A preparation method of a wear-resistant corrosion-resistant carbide ceramic coating specifically comprises the following steps:
step 1: pretreatment of metal substrates
The Q235 steel is firstly polished to remove oxide skin on the surface by using No.320 abrasive paper, and then sequentially polished to be smooth and consistent in roughness on the surface of the metal substrate by using No.600 abrasive paper and No.800 abrasive paper respectively. And (3) putting the polished metal matrix into absolute ethyl alcohol for ultrasonic treatment for 10min, and removing the residual abrasive particles and other pollution stains on the surface of the metal matrix. And (3) drying the metal matrix subjected to ultrasonic treatment in a drying oven at 60 ℃ for 20min so as to completely volatilize the absolute ethyl alcohol on the surface of the metal matrix and ensure that the metal surface is clean and pollution-free, and finishing pretreatment of the matrix according to the requirements to obtain a clean matrix.
Step 2: preparation of impregnation liquid and impregnation of metal matrix
Push button
6.05g of PCS was weighed and dissolved in 11mL of chloroform, sealed with a preservative film because chloroform is volatile, stirred for 15min to dissolve PCS in chloroform sufficiently to obtain a PCS solution, and then M was addedd＝(MInertia device+Mg+Mf) 0.04 weight of 0.211g of castor oil phosphate, adding dispersant to the PCS solution obtained above, stirring for 3min to disperse the dispersant uniformly in the solution, the solution obtained at this time being called solution A, and
2.723g of SiC powder and 0.424g of Al were weighed out separately2O3Fiber, 2.118g ST 880. 2.723g of SiC powder is added into the solution A, stirred for 3min, and then 2.118g of ST880 and 0.424g of Al are respectively added2O3Stirring the fiber for 4h to fully disperse the three fillers in the solution A to form a solution B, wherein the solution B is preparedAnd preparing an immersion liquid, namely suspending the metal substrate pretreated according to the requirements on an immersion pulling machine, performing immersion at a descending speed of 1000 mu m/s and a pulling speed of 1000 mu m/s, standing the substrate in the immersion liquid for 4min, and circulating for 2 times.
And step 3: the cross-linking and pyrolysis of the coating can prepare a wear-resistant and corrosion-resistant carbide ceramic coating
And (3) placing the substrate soaked according to the requirements in a blast drying oven, heating to 180 ℃ at the heating rate of 2 ℃/min in the air atmosphere, preserving the heat for 3h, and cooling to room temperature at the cooling rate of 2 ℃/min, thus completing the crosslinking process of the coating and obtaining the metal substrate with the crosslinked surface coating. And (3) placing the substrate with the crosslinked surface coating in a vacuum tube furnace, changing the air in the furnace tube into argon, heating to 400 ℃ at the heating rate of 3 ℃/min, then heating to 900 ℃ at the heating rate of 2 ℃/min, preserving the heat for 1h, cooling to 400 ℃ at the cooling rate of 2 ℃/min, and then cooling to room temperature at the cooling rate of 3 ℃/min, thus completing the pyrolysis process of PCS (polycarbonate-coated ceramic), forming a compact wear-resistant corrosion-resistant SiC ceramic coating on the surface of the metal substrate, wherein the thickness of the prepared coating is about 30 mu m.
Example 4
A preparation method of a wear-resistant corrosion-resistant carbide ceramic coating specifically comprises the following steps:
step 1: pretreatment of substrates
The Q235 steel is firstly polished to remove oxide skin on the surface by using No.320 abrasive paper, and then sequentially polished to be smooth and consistent in roughness on the surface of the metal substrate by using No.600 abrasive paper and No.800 abrasive paper respectively. And (3) putting the polished metal matrix into absolute ethyl alcohol for ultrasonic treatment for 10min, and removing the residual abrasive particles and other pollution stains on the surface of the metal matrix. And (3) drying the metal matrix subjected to ultrasonic treatment in an oven at 60 ℃ for 10min so as to completely volatilize the absolute ethyl alcohol on the surface of the metal matrix and ensure that the metal surface is clean and pollution-free, and finishing pretreatment of the matrix according to the requirements to obtain a clean matrix.
Step 2: preparation of impregnation liquid and impregnation of metal matrix
Push button
6.05g of PCS was weighed and dissolved in 11mL of toluene, the toluene was volatile, the solution was sealed with a preservative film, stirred for 10min to dissolve PCS in toluene sufficiently to obtain a PCS solution, and then M was addedd＝(MInertia device+Mg+Mf) 0.03 weighing 0.133g of castor oil phosphate, adding dispersant to the PCS solution obtained above, stirring for 5min to disperse the dispersant uniformly in the solution, the solution obtained at this time being called solution A, and
3.025g of SiO were weighed separately2Powder, 0.484g of SiC fibers, and 0.908g of ST 880. Adding 3.025g SiO into the solution A2And (3) stirring the powder for 3min, then respectively adding 0.908g of ST880 and 0.484g of SiC fiber, stirring for 5h, fully dispersing the three fillers in the solution A to form a solution B, wherein the solution B is the prepared impregnation solution, suspending the metal matrix pretreated according to the requirements on an impregnation pulling machine, impregnating at a descending speed of 1000 mu m/s and a pulling speed of 1000 mu m/s, standing the matrix in the impregnation solution for 2min, and circulating for 3 times.
And step 3: the cross-linking and pyrolysis of the coating can prepare a wear-resistant and corrosion-resistant carbide ceramic coating
And (3) placing the substrate soaked according to the requirements in a blast drying oven, heating to 190 ℃ at the heating rate of 1 ℃/min in the air atmosphere, preserving the heat for 2h, and cooling to room temperature at the cooling rate of 1 ℃/min, thus completing the crosslinking process of the coating and obtaining the metal substrate with the crosslinked surface coating. And (3) placing the substrate with the crosslinked surface coating in a vacuum tube furnace, changing the air in the furnace tube into argon, heating to 350 ℃ at the heating rate of 3 ℃/min, then heating to 850 ℃ at the heating rate of 2 ℃/min, preserving the heat for 2h, cooling to 350 ℃ at the cooling rate of 2 ℃/min, and then cooling to room temperature at the cooling rate of 3 ℃/min, thus completing the pyrolysis process of PCS (polycarbonate-coated ceramic), forming a compact wear-resistant corrosion-resistant SiC ceramic coating on the surface of the metal substrate, wherein the thickness of the prepared coating is about 45 mu m.
Example 5
A preparation method of a wear-resistant corrosion-resistant carbide ceramic coating specifically comprises the following steps:
step 1: pretreatment of substrates
The Q235 steel is firstly polished to remove oxide skin on the surface by using No.320 abrasive paper, and then sequentially polished to be smooth and consistent in roughness on the surface of the metal substrate by using No.600 abrasive paper and No.800 abrasive paper respectively. And (3) putting the polished metal matrix into absolute ethyl alcohol for ultrasonic treatment for 10min, and removing the residual abrasive particles and other pollution stains on the surface of the metal matrix. And (3) drying the metal matrix subjected to ultrasonic treatment in a drying oven at 60 ℃ for 15min so as to completely volatilize the absolute ethyl alcohol on the surface of the metal matrix and ensure that the metal surface is clean and pollution-free, and finishing pretreatment of the matrix according to the requirements to obtain a clean matrix.
Step 2: preparation of impregnation liquid and impregnation of metal matrix
Push button
Weighing 5.5g of PCS to dissolve in 11mL of tetrahydrofuran, sealing the opening of the opening with a preservative film because the tetrahydrofuran is volatile, stirring for 10min to fully dissolve the PCS in the tetrahydrofuran to obtain a PCS solution, and then adding M to the PCS solutiond＝(MInertia device+Mg+Mf) 0.03 weigh 0.134g of Pasteur dispersant (model Efka FA 4663AN), add dispersant to the PCS solution obtained above, stir for 5min to disperse dispersant uniformly in the solution, the solution obtained at this time is called solution A, then
2.75g of SiC powder, 0.33g of SiC fibers, and 1.375g of ST880 were weighed out, respectively. Adding 2.75g of SiC powder into the solution A, stirring for 3min, then respectively adding 1.375g of ST880 and 0.33g of SiC fiber, stirring for 5h, fully dispersing the three fillers into the solution A to form a solution B, wherein the solution B is the prepared impregnation solution, suspending the metal matrix pretreated according to the requirements on an impregnation drawing machine, impregnating at a descending speed of 800 mu m/s and a drawing speed of 800 mu m/s, standing the matrix in the impregnation solution for 2min, and circulating for 1 time.
And step 3: the cross-linking and pyrolysis of the coating can prepare a wear-resistant and corrosion-resistant carbide ceramic coating
And (3) placing the substrate soaked according to the requirements in a blast drying oven, heating to 180 ℃ at the heating rate of 1.5 ℃/min in the air atmosphere, preserving the heat for 2.5 hours, and cooling to room temperature at the cooling rate of 1.5 ℃/min, thus completing the crosslinking process of the coating and obtaining the metal substrate with the crosslinked surface coating. And (3) placing the substrate with the crosslinked surface coating in a vacuum tube furnace, changing the air in the furnace tube into argon, heating to 420 ℃ at the heating rate of 3.5 ℃/min, then heating to 880 ℃ at the heating rate of 2.5 ℃/min, preserving the heat for 1.5h, cooling to 420 ℃ at the cooling rate of 2.5 ℃/min, and then cooling to room temperature at the cooling rate of 3.5 ℃/min, thus completing the pyrolysis process of PCS, and forming a compact wear-resistant SiC corrosion-resistant ceramic coating on the surface of the metal substrate, wherein the thickness of the prepared coating is about 15 mu m.
Example 6:
a preparation method of a wear-resistant corrosion-resistant carbide ceramic coating specifically comprises the following steps:
step 1: pretreatment of substrates
The Q235 steel is firstly polished to remove oxide skin on the surface by using No.320 abrasive paper, and then sequentially polished to be smooth and consistent in roughness on the surface of the metal substrate by using No.600 abrasive paper and No.800 abrasive paper respectively. And (3) putting the polished metal matrix into absolute ethyl alcohol for ultrasonic treatment for 10min, and removing the residual abrasive particles and other pollution stains on the surface of the metal matrix. And (3) drying the metal matrix subjected to ultrasonic treatment in an oven at 60 ℃ for 10min so as to completely volatilize the absolute ethyl alcohol on the surface of the metal matrix and ensure that the metal surface is clean and pollution-free, and finishing pretreatment of the matrix according to the requirements to obtain a clean matrix.
Step 2: preparation of impregnation liquid and impregnation of metal matrix
Push button
5.5g PCS was weighed and dissolved in 11mL xylene, since xylene was volatile, the mixture was sealed with a preservative film and stirred for 10min to dissolve PCS in dimethyl sufficientlyIn benzene to give a PCS solution, then as Md＝(MInertia device+Mg+Mf) 0.03 weighing 0.15g of Pasteur dispersant (model Efka FA 4663AN), adding the dispersant to the PCS solution obtained above, stirring for 5min to disperse the dispersant uniformly in the solution, the solution obtained at this time being called solution A, and then
2.75g of SiC powder and 0.33g of ZrO were weighed out separately2Fiber, 1.925g ST 880. Adding 2.75g SiC powder into the solution A, stirring for 3min, and then adding 1.925g ST880 and 0.33g ZrO respectively2Stirring the fiber for 5.5h to fully disperse the three fillers in the solution A to form a solution B, wherein the solution B is the prepared impregnation liquid, suspending the metal matrix pretreated according to the requirements on an impregnation drawing machine, impregnating at a descending speed of 800 mu m/s and a drawing speed of 800 mu m/s, standing the matrix in the impregnation liquid for 3min, and circulating for 1 time.
And step 3: the cross-linking and pyrolysis of the coating can prepare a wear-resistant and corrosion-resistant carbide ceramic coating
And (3) placing the substrate soaked according to the requirements in a blast drying oven, heating to 190 ℃ at the heating rate of 1 ℃/min in the air atmosphere, preserving the heat for 2h, and cooling to room temperature at the cooling rate of 1 ℃/min, thus completing the crosslinking process of the coating and obtaining the metal substrate with the crosslinked surface coating. And (3) placing the substrate with the crosslinked surface coating in a vacuum tube furnace, changing the air in the furnace tube into argon, heating to 400 ℃ at the heating rate of 3 ℃/min, then heating to 900 ℃ at the heating rate of 2 ℃, preserving the heat for 1h, cooling to 400 ℃ at the cooling rate of 2 ℃/min, and then cooling to room temperature at the cooling rate of 3 ℃/min, thus completing the pyrolysis process of PCS, forming a compact wear-resistant corrosion-resistant SiC ceramic coating on the surface of the metal substrate, wherein the thickness of the prepared coating is about 15 mu m.
In summary, with the specific embodiments of the present invention, it can be seen that the wear-resistant corrosion-resistant carbide ceramic coating and the preparation method thereof disclosed in the present invention have good continuity and compactness, and the coating is well bonded with the surface of the substrate. The SiC ceramic coating can play the roles of abrasion resistance and corrosion resistance. The preparation of the wear-resistant corrosion-resistant SiC ceramic coating comprises the steps of pretreatment of a matrix, preparation of impregnation liquid, impregnation of the pretreated metal matrix, and crosslinking and pyrolysis of the impregnated coating. The wear-resistant corrosion-resistant SiC ceramic coating provided by the invention is a wear-resistant corrosion-resistant SiC coating which has good bonding property with the surface of a metal matrix, and the preparation method provided by the invention adopts a dipping and pulling method and a precursor cracking method to prepare the SiC coating, is convenient and fast in operation process, is suitable for metal matrixes with various shapes, has high economic benefit, and is suitable for industrial batch production. By adding a certain amount of inert filler and fiber filler with a certain size range into the coating, the SiC Precursor (PCS) can be effectively inhibited from generating large shrinkage during cracking; furthermore, the glass filler with certain initial melting temperature is added into the system, so that cracks generated when the coating is cracked are further filled by the glass filler which is gradually melted in the cracking process, the compactness of the coating is further increased, the corrosion resistance of the coating is effectively improved, the problems of large shrinkage of the SiC coating prepared by the existing dipping method process and poor combination between the coating prepared by the existing dipping method process and the matrix are solved, the compactness and continuity of the SiC ceramic coating are improved, and the corrosion resistance of the SiC ceramic coating is effectively improved.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. A preparation method of a wear-resistant corrosion-resistant carbide ceramic coating is characterized in that a dipping and pulling method is adopted to dip a substrate in a dipping solution to obtain a dipped substrate; sequentially carrying out cross-linking treatment and pyrolysis treatment on the impregnated matrix to prepare a wear-resistant corrosion-resistant carbide ceramic coating on the matrix;
the impregnation liquid comprises a SiC precursor, a SiC precursor solvent, an inert filler, a glass filler, a fiber filler and a dispersing agent.
2. The method for preparing a wear and corrosion resistant carbide ceramic coating according to claim 1, wherein the SiC precursor is polycarbosilane; the SiC precursor solvent is xylene, toluene, tetrahydrofuran or chloroform.
3. The method for preparing a wear-resistant and corrosion-resistant carbide ceramic coating according to claim 1, wherein the inert filler is SiC powder or SiO2Powder;
the glass filler is commercial ST880 powder;
the fibrous filler is a carbide fiber or an oxide fiber.
4. The method for preparing a wear and corrosion resistant carbide ceramic coating according to claim 3, wherein the fibrous filler is SiC fibers, Al2O3Fibres or ZrO2A fiber.
5. The method for preparing the wear-resistant and corrosion-resistant carbide ceramic coating according to claim 1, wherein the impregnating solution is prepared according to the following formula:
a) the proportion of the SiC precursor to the SiC precursor solvent is as follows:
wherein: mpMass/g, V of SiC precursors-volume/mL of SiC precursor solvent;
b) the proportion of the SiC precursor to the inert filler, the glass filler and the fiber filler is as follows:
wherein: mpMass/g, M of SiC precursorInertia deviceMass/g, M of inert fillergMass/g, M of glass fillerf-mass of fibrous filler/g;
c) the amount of dispersant is calculated as follows:
Md＝(Minertia device+Mg+Mf)×0.02～0.04；
Wherein: mInertia deviceMass/g, M of inert fillergMass/g, M of glass fillerdMass of dispersant/g, Mf-mass of fibrous filler/g.
6. The method for preparing the wear-resistant and corrosion-resistant carbide ceramic coating according to claim 1, wherein the preparation process of the impregnating solution comprises the following steps: firstly, dissolving a SiC precursor in a SiC precursor solvent to obtain a precursor solution, then uniformly dispersing a dispersing agent in the obtained precursor solution to obtain a solution A, and finally uniformly dispersing a fiber filler, an inert filler and a glass filler in the obtained solution A to obtain an impregnation solution.
7. The method for preparing the wear-resistant and corrosion-resistant carbide ceramic coating according to claim 1, wherein the dip-draw method comprises the following steps: dipping the substrate at a descending speed of 800-1500 μm/s and a pulling speed of 800-1500 μm/s, wherein the substrate is kept in the dipping solution for 2-5 min, and the cycle is 1-3 times.
8. The method for preparing the wear-resistant and corrosion-resistant carbide ceramic coating according to claim 1, wherein the process parameters of the cross-linking treatment comprise: heating to 180-200 ℃ at a heating rate of 1-2 ℃/min, preserving heat for 2-3 h, and cooling to room temperature at a cooling rate of 1-2 ℃/min.
9. The method for preparing a wear-resistant and corrosion-resistant carbide ceramic coating according to claim 1, wherein the process parameters of the pyrolysis treatment comprise: heating to 350-450 ℃ at a heating rate of 3-4 ℃/min, heating to 850-950 ℃ at a heating rate of 2-3 ℃/min, preserving heat for 1-2 h, cooling to 350-450 ℃ at a cooling rate of 2-3 ℃/min, and cooling to room temperature at a cooling rate of 3-4 ℃/min.
10. A wear and corrosion resistant carbide ceramic coating produced by the method of any one of claims 1 to 9.
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