CN111676469A - SiC/Al prepared by laser cracking polycarbosilane precursor2O3Method for multiphase ceramic coating - Google Patents
SiC/Al prepared by laser cracking polycarbosilane precursor2O3Method for multiphase ceramic coating Download PDFInfo
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- CN111676469A CN111676469A CN202010400617.8A CN202010400617A CN111676469A CN 111676469 A CN111676469 A CN 111676469A CN 202010400617 A CN202010400617 A CN 202010400617A CN 111676469 A CN111676469 A CN 111676469A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
- C23C18/143—Radiation by light, e.g. photolysis or pyrolysis
Abstract
The invention relates to a method for preparing SiC/Al by using a polycarbosilane precursor through laser pyrolysis2O3A method for complex phase ceramic coating. The polycarbosilane is used as a precursor, SiC particles are used as inert filler, and Al powder is used as active filler, so that the volume shrinkage and the porosity of the multiphase ceramic coating are reduced. The method comprises the steps of preparing precursor slurry containing inert filler and active filler, coating the precursor slurry on the surface of a treated base material by using a dipping-lifting, brushing or spraying method, and carrying out laser scanning on the coating under the protection of inert gas to realize ceramic conversion to obtain SiC/Al2O3Complex phase ceramic coating. The invention has the advantages of simplicity, short preparation period, high efficiency, low cost and high benefit, the shape and the tissue performance of the matrix are not negatively influenced by laser scanning, the formation of gaps in the ceramic coating is effectively inhibited by adding the inert filler and the active filler, the surface of the ceramic coating is smooth, the porosity is low, and the ceramic coating has higher hardness and excellent wear-resisting and friction-reducing properties. The invention solves the problem of onlyIron-based metal materials are difficult to reliably serve under certain working conditions.
Description
Technical Field
The invention relates to a method for preparing SiC/Al with excellent wear resistance, oxidation resistance and mechanical properties on the surface of iron-based metal by utilizing laser pyrolysis2O3A method of complex phase ceramic coating belongs to the advanced ceramic coating preparation field.
Background
The continuous and high-speed development of high-tech and industrial modernization makes the working conditions of various mechanical parts increasingly strict, and the materials are required to have the performances of high temperature resistance, corrosion resistance, vibration resistance, fatigue resistance, temperature shock resistance, scouring resistance and the like, so that the simple metal materials are difficult to meet the requirements. The preparation of high-performance coating materials on the surfaces of metal parts and endowing the metal parts with special functions has become an effective way for solving the problem of reliable service of the metal parts under severe working conditions. Aiming at different service conditions and failure characteristics of parts, different ceramic material systems are selected, a layer of uniform, compact and firmly combined composite protective coating is prepared on the surface of a metal matrix by adopting a proper process technology, the higher strength, toughness and good manufacturability of a metal material are organically combined with the excellent wear resistance, corrosion resistance and chemical stability of the ceramic material, and the service life of the metal part can be greatly prolonged. The non-oxide composite material has become an important direction for the development of composite materials, a second phase is added into a single-phase material to prepare the composite material, the advantages of all substances among the materials are complementary, the performance of the material can be effectively improved, and SiC ceramic and Al are mixed2O3The two ceramic materials are compounded to obtain SiC/Al with excellent mechanical property2O3Complex phase ceramic coating.
At present, the preparation methods of ceramic coatings mainly include high-speed flame thermal spraying, plasma thermal spraying, chemical vapor deposition, sol-gel method, electroheating method, precursor conversion ceramic method and the like, wherein the precursor conversion ceramic method is a novel method for in-situ preparation of advanced ceramic coatings. The precursor conversion ceramic method utilizes the characteristics of good fluidity, formability, processability, structure designability and the like of a precursor polymer to coat precursor slurry on a substrate material to form a ceramic coating on the surface of the substrate material. In the traditional precursor ceramic conversion method, a precursor is put in a heating furnace to be pyrolyzed so as to be converted into a ceramic coating, but the pyrolysis time is long, the energy consumption is large, and the performance of a substrate material is influenced. The laser has the characteristics of high energy density, controllable power, rapid melting and solidification, rapid laser cracking, uniform heating and the like. Meanwhile, the laser has unique precision and local heat action, and can be used for preparing ceramic coatings on the surfaces of materials with low melting points, such as high polymer materials or metal aluminum. Therefore, the laser is used as a heat source for cracking the polymer precursor, and the rapid and in-situ preparation of the high-quality ceramic coating on the surface of the polymer precursor without influencing the performance of the matrix material is a new way for preparing the advanced ceramic coating by a precursor-to-ceramic method.
In the precursor conversion ceramic process, residual stress is generated in the ceramic coating along with the formation of void shrinkage caused by density change during the conversion of the precursor polymer to the ceramic coating, causing cracks in the prepared coating. The inert filler and the active filler are added into the precursor, so that the volume shrinkage in the cracking process of the precursor polymer can be inhibited and compensated, and the porosity of the coating is reduced. The mass and the volume of the inert filler SiC particles are not changed in the precursor cracking process, and the volume shrinkage of the ceramic coating can be inhibited. The active Al powder is converted from simple substance Al to Al2O3The volume is expanded in the process, the volume shrinkage generated in the process of converting the polymer into the ceramic can be completely or partially compensated, and the oxygen element in the system can be absorbed, so that the influence of the mechanical property and the thermal stability of the oxygen ceramic coating is reduced.
Disclosure of Invention
The invention provides a method for preparing SiC/Al with low cost and high benefit2O3A new method of multiple phase ceramic coating. The method comprises the steps of utilizing a precursor ceramic conversion method, utilizing laser as a cracking heat source, utilizing nano SiC particles as inert filler and metal Al powder as active filler, coating a layer of ceramic precursor polymer or slurry formed by compounding a second phase and the precursor polymer on the surface of a metal matrix material, drying and curing the coating, and then carrying out laser scanning on the coating under the protection of inert gas to form a layer of compact SiC/Al with proper thickness2O3The multiphase ceramic coating realizes the in-situ preparation of the multiphase ceramic coating on the surface of the metal part, so that the metal part has the strength and toughness of a metal material, has the advantages of high temperature resistance, corrosion resistance and wear resistance of a ceramic material, and greatly prolongs the service life of the metal part.
The invention aims to provide SiC/Al2O3An effective preparation method of a complex phase ceramic coating.
SiC/Al prepared by converting precursor into ceramic by using laser as heating source2O3The method for the complex phase ceramic coating is characterized by comprising the following steps:
(1) pretreating the surface of the substrate by adopting a mechanical or electrochemical method, then decontaminating and cleaning the surface of the substrate by utilizing acetone and distilled water, and drying for later use;
(2) preparing precursor slurry: adding inert filler SiC powder and active filler Al powder into a polycarbosilane precursor, adding a solvent, stirring and dispersing, and grinding by using a ball mill to obtain uniform precursor slurry;
(3) preparing a precursor coating: coating the precursor slurry on the surface of the processed substrate in a manner of dipping-lifting, brushing or spraying;
(4) curing a precursor coating: putting the precursor coating coated on the surface of the substrate into a heating furnace, heating to 200 ℃ in the air, and preserving heat for 2h for curing;
(5) and (3) cracking: under the protection of inert gasScanning the solidified precursor coating by continuous laser, cracking the coating to obtain SiC/Al2O3Complex phase ceramic coating.
In the step (1), the matrix is one of high-speed steel, hard alloy, metal ceramic or ceramic;
in the step (1), the pretreatment of the surface of the base material by a mechanical or electrochemical method refers to surface sand blasting, organic solvent soaking, ultrasonic treatment, surface anodic oxidation treatment and micro-arc oxidation treatment or a combination thereof.
In the step (2), the molecular weight of the polycarbosilane is 1000-2000.
In the step (2), the granularity of the Al powder is 50-100 nm; the granularity of the SiC nano powder is 10-100 nm.
In the step (2), the mass fraction of the Al powder relative to the polycarbosilane is 10-60%, and the mass fraction of the SiC nano powder relative to the polycarbosilane is 10-20%.
In the step (2), the solvent is xylene.
In the step (5), the inert shielding gas is argon or nitrogen, and the flow rate is 300E
500mL/min。
In the step (5), the laser is selected as a continuous high-power semiconductor laser, the wavelength is 980nm, the power is 200-1000W, the working distance is 300 +/-10 mm, the scanning speed is 5-30 mm/s, the spot size is (2-16) × (1.5-4) mm, and the scanning lap joint rate is 3% -5%.
The invention provides a method for preparing SiC/Al2O3The process flow of the complex phase ceramic coating is shown in figure 1.
Compared with the existing ceramic coating, the preparation technology of the complex phase ceramic coating has the following advantages:
(1) the precursor in the precursor conversion ceramic method is rich in variety, heterogeneous elements can be uniformly mixed with the precursor molecule level through the molecular design of the organic precursor, and the components, the structure and the performance of the ceramic coating can be controlled;
(2) the precursor slurry can penetrate into the substrate material to form a gradient coating on the coating/substrate interface, so that the interface stress is relieved, and the coating/substrate bonding strength is improved.
(3) The precursor slurry is in a liquid state, and can be used for preparing composite material parts with complex shapes and near sizes by means of additive remanufacturing technology.
(4) The laser is used as a heat source to be applied to a precursor ceramic conversion method, the laser energy is concentrated, the flexibility is good, the cracking process is rapid, the processing efficiency is high, and the processing mode is flexible. Meanwhile, the heat affected zone is small, and the composition and the performance of the base material are not affected.
(5) The addition of the inert filler SiC particles and the active Al powder can completely or partially compensate the volume shrinkage generated in the process of converting the precursor polymer into the ceramic, reduce the porosity of the coating, inhibit the generation of cracks and realize the high-quality SiC/Al2O3Controllable preparation of the complex phase ceramic coating.
(6) The multiphase ceramic coating has excellent mechanical property, SiC/Al2O3The hardness of the complex phase ceramic coating can reach 1470HV, and the friction coefficient is only 0.27 at the minimum.
Drawings
FIG. 1 shows that SiC/Al is prepared by taking SiC particles as inert filler and Al powder as active filler according to the invention2O3Schematic representation of complex phase ceramic coatings.
FIG. 2 shows SiC/Al prepared by the present invention2O3Complex phase ceramic coating surface topography.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
Example 1
100g of polycarbosilane with the molecular weight of 1000-2000 is taken, 10g of SiC nano powder with the particle size of 20nm is taken as Al powder with the mass fraction of 30 percent relative to the polycarbosilane, 120mL of p-xylene solvent is added after stirring, the mixture is stirred and dispersed, and is ground into uniform slurry by using a ball mill, the substrate material is 45 steel, the size is 10mm × 20mm × 1.0.0 mm, the substrate material is ground and polished, ultrasonic cleaning is carried out, then distilled water and acetone are used for washing and drying, the obtained precursor slurry is coated on the substrate material by using a dipping-pulling method, and the speed of dipping and pulling is controlled at the speed of dipping and pulling4cm·min-1. Putting the precursor coating coated on the surface of the substrate into a heating furnace, and heating at 1 ℃ for min in air-1Heating to 200 ℃, preserving heat for 2h, curing, scanning the cured precursor coating by laser scanning, wherein the laser wavelength is 980nm, the laser power is 500W, the spot size is 14mm × 2mm, the working distance is 300mm, the scanning speed is 10mm/s, the scanning lap joint rate is 4%, nitrogen is used as protective gas, the nitrogen flow is 500mL/min, and cooling to room temperature is carried out after laser scanning, thus obtaining the SiC/Al2O3Complex phase ceramic coating. And (3) performing performance test on the prepared ceramic coating, and respectively testing the hardness and the friction coefficient of the composite coating by adopting a Vickers hardness tester and a friction and wear tester, wherein the hardness and the friction coefficient are 1340HV and 0.31 respectively.
Example 2
100g of polycarbosilane with the molecular weight of 1000-2000 is taken, 10g of SiC nano powder with the particle size of 20nm is taken as Al powder with the mass fraction of 40 percent relative to the polycarbosilane, 120mL of p-xylene solvent is added after stirring, the mixture is stirred and dispersed, and is ground by a ball mill to form uniform slurry, the base material is 45 steel, the size is 10mm × 20mm, the size is × 1.0.0 mm, the ultrasonic cleaning is carried out after grinding and polishing, then the washing is carried out by distilled water and acetone, the drying is carried out, the obtained precursor slurry is coated on the base material by a dipping-pulling method, the dipping and pulling speed is 4 cm-min-1. Putting the precursor coating coated on the surface of the substrate into a heating furnace, and heating at 1 ℃ for min in air-1Heating to 200 ℃, preserving heat for 2h, curing, scanning the cured precursor coating by laser scanning, wherein the laser wavelength is 980nm, the laser power is 500W, the spot size is 14mm × 2mm, the working distance is 300mm, the scanning speed is 10mm/s, the scanning lap joint rate is 4%, nitrogen is used as protective gas, the nitrogen flow is 500mL/min, and cooling to room temperature is carried out after laser scanning, thus obtaining the SiC/Al2O3Complex phase ceramic coating. And (3) performing performance test on the prepared ceramic coating, and respectively testing the hardness and the friction coefficient of the composite coating by adopting a Vickers hardness tester and a friction and wear tester, wherein the hardness and the friction coefficient are 1420HV and 0.27 respectively.
The following is further described with reference to the accompanying drawings.
FIG. 2 shows SiC/Al2O3SEM photographs of the interface (a) and the surface (b) of the complex phase ceramic coating show that as can be seen from figure 2, the surface of the ceramic coating is relatively flat and compact, no defects such as obvious cracks, holes and the like exist, and the interface combination of the ceramic coating and the substrate is good.
Example 3
100g of polycarbosilane with the molecular weight of 1000-2000 is taken, 10g of SiC nano powder with the particle size of 20nm is taken as Al powder with the mass fraction of 40 percent relative to the polycarbosilane, 120mL of p-xylene solvent is added after stirring, the mixture is stirred and dispersed, and is ground by a ball mill to form uniform slurry, the base material is 45 steel, the size is 10mm × 20mm, the size is × 1.0.0 mm, the ultrasonic cleaning is carried out after grinding and polishing, then the washing is carried out by distilled water and acetone, the drying is carried out, the obtained precursor slurry is coated on the base material by a dipping-pulling method, the dipping and pulling speed is 4 cm-min-1. Putting the precursor coating coated on the surface of the substrate into a heating furnace, and heating at 1 ℃ for min in air-1Heating to 200 ℃, preserving heat for 2h, curing, scanning the cured precursor coating by laser scanning, wherein the laser wavelength is 980nm, the laser power is 500W, the spot size is 14mm × 2mm, the working distance is 300mm, the scanning speed is 10mm/s, the scanning lap joint rate is 4%, nitrogen is used as protective gas, the nitrogen flow is 500mL/min, and cooling to room temperature is carried out after laser scanning, thus obtaining the SiC/Al2O3Complex phase ceramic coating. And (3) performing performance test on the prepared ceramic coating, and respectively testing the hardness and the friction coefficient of the composite coating by adopting a Vickers hardness tester and a friction and wear tester, wherein the hardness and the friction coefficient are 1470HV and 0.28 respectively.
The hardness and the friction coefficient of a 45 steel matrix are 480HV and 0.52 respectively, and the complex phase ceramic coating prepared by the method is compact, is well combined with the matrix, and has higher hardness and excellent wear resistance.
Claims (7)
1. SiC/Al prepared by laser cracking polycarbosilane precursor2O3The method for complex phase ceramic coating is characterized by comprising the following steps:
(1) pretreating the surface of the substrate by adopting a mechanical or electrochemical method, then decontaminating and cleaning the surface of the substrate by utilizing acetone and distilled water, and drying for later use;
(2) preparing precursor slurry: adding inert filler SiC powder and active filler Al powder into a polycarbosilane precursor, adding a solvent, stirring and dispersing, and grinding by using a ball mill to obtain uniform precursor slurry; the mass fraction of the Al powder relative to the polycarbosilane is 10-60%, and the mass fraction of the SiC nano powder relative to the polycarbosilane is 10-20%;
(3) preparing a precursor coating: coating the precursor slurry on the surface of the processed substrate in a manner of dipping-lifting, brushing or spraying;
(4) curing a precursor coating: putting the precursor coating coated on the surface of the substrate into a heating furnace, heating to 200 ℃ in the air, and preserving heat for 2h for curing;
(5) and (3) cracking: scanning the solidified precursor coating by adopting continuous laser under the protection of inert gas, cracking the coating to obtain SiC/Al2O3The multiphase ceramic coating is characterized in that a continuous high-power semiconductor laser is selected as the laser, the wavelength is 980nm, the power is 200-1000W, the working distance is 300 +/-10 mm, the scanning speed is 5-30 mm/s, the spot size is (2-16) × (1.5-4) mm, and the scanning lap joint rate is 3% -5%.
2. The method of claim 1, wherein: in the step (1), the substrate is one of high-speed steel, hard alloy, metal ceramic or ceramic.
3. The method of claim 1, wherein: in the step (1), the pretreatment of the surface of the base material by a mechanical or electrochemical method refers to surface sand blasting, organic solvent soaking, ultrasonic treatment, surface anodic oxidation treatment and micro-arc oxidation treatment or a combination thereof.
4. The method of claim 1, wherein: in the step (2), the molecular weight of the polycarbosilane is 1000-2000.
5. The method of claim 1, wherein: in the step (2), the granularity of the Al powder is 50-100 nm; the granularity of the SiC nano powder is 10-100 nm.
6. The method of claim 1, wherein: in the step (2), the solvent is xylene.
7. The method of claim 1, wherein: the inert protective gas is argon or nitrogen, and the flow rate is controlled to be 300-500 mL/min.
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CN113957379A (en) * | 2021-10-26 | 2022-01-21 | 西安热工研究院有限公司 | N-SiC/Al2O3Nano composite corrosion-resistant coating and preparation method thereof |
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