CN116589281A - Silicon carbide composite material member and preparation process method thereof - Google Patents

Silicon carbide composite material member and preparation process method thereof Download PDF

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CN116589281A
CN116589281A CN202310564239.0A CN202310564239A CN116589281A CN 116589281 A CN116589281 A CN 116589281A CN 202310564239 A CN202310564239 A CN 202310564239A CN 116589281 A CN116589281 A CN 116589281A
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silicon carbide
resin
composite material
carbide composite
siliconizing
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王东
黄海兴
石威
李伟强
王强
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Shandong Huamei New Material Technology Co ltd
Weifang Huamei Intelligent Technology Co ltd
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Shandong Huamei New Material Technology Co ltd
Weifang Huamei Intelligent Technology Co ltd
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Abstract

The invention discloses a preparation method of a silicon carbide composite material component, which comprises the following steps: s1: selecting a silicon carbide material as a matrix material, optionally selecting a carbon material as an auxiliary material, taking one or more of phenolic resin, furan resin, PVA or PVB as a binder, and forming a first blank with a required structure by adopting an additive manufacturing technology; s2: the first green body is immersed in a resin solution. The invention adopts a 3D printing method, also called additive manufacturing, and solves the problems of preparation of silicon carbide composite material components for large-scale pumps with complex structures by adopting an improved process, thereby being beneficial to expanding the application field and realizing industrialized mass production.

Description

Silicon carbide composite material member and preparation process method thereof
Technical Field
The invention relates to the technical field of advanced manufacturing and additive manufacturing, in particular to a silicon carbide composite material component for a 3D printing pump, a preparation method thereof and a pump comprising the component.
Background
The slurry pump is a pump for conveying a solid-liquid mixture, and is widely applied to the technical fields of mines, power plants, dredging, metallurgy, chemical industry, building materials and the like, and is used for conveying slurry containing corrosive solid particles. The application working condition is generally severe, the slurry with abrasiveness and corrosiveness is easy to damage the overflow part of the slurry pump, the sheath materials of the existing slurry pump mainly comprise A49, A33, cr30, A05, A07, duplex stainless steel, rubber R55 and the like, but the corrosion resistance and the wear resistance of the materials are relatively low, so that the service life of the heavy slurry pump is shortened, the replacement is frequent, the time and the labor are wasted, and the maintenance cost of equipment is increased. The ceramic slurry pump is a slurry pump with a ceramic sheath, and can be used for replacing the original rubber sheath slurry pump, metal sheath slurry pump and the like. The ceramic slurry pump has the greatest characteristics of wear resistance and corrosion resistance, and the wear resistance and the corrosion resistance are far higher than those of alloy pumps and rubber pumps. Through multiple tests and data feedback of metal ore dressing plants for many years, the service life of the ceramic slurry pump is generally 3-6 times that of a high-chromium alloy pump under the same working condition. At present, the most adopted ceramic slurry pump ceramic materials are mainly made of silicon carbide materials, the processes of various manufacturers are different and mainly comprise resin-bonded silicon carbide and sintered silicon carbide, and compared with high-chromium steel and dual-phase steel, the silicon carbide materials are lower in price, so that the ceramic slurry pump has great economic advantages compared with the alloys of the prior art in raw material price.
The Mohs hardness of the silicon carbide is 9.5, which is inferior to the hardest substance diamond in nature (the hardness is 10), and the silicon carbide has the advantages of good chemical property stability, high heat conductivity coefficient, small thermal expansion coefficient and good wear resistance, and is mainly used for four application fields of silicon carbide ceramics, namely: structural ceramics, advanced refractory materials, abrasives and metallurgical raw materials. The silicon carbide material has the characteristics of being suitable for the working conditions of abrasion and corrosion, but the silicon carbide ceramic is fragile and has poor impact resistance, cannot bear the impact of solid particles in a slurry pump, needs to improve the impact resistance of the silicon carbide material through technological improvement, solves the problem of the fragile silicon carbide material, and is successfully used in the slurry pump.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a silicon carbide composite material component, the silicon carbide composite material component prepared by the method and a pump comprising the component.
The invention provides a preparation method of a silicon carbide composite material component, which comprises the following steps: s1: selecting a silicon carbide material as a matrix material, optionally selecting a carbon material as an auxiliary material, and taking one or more of phenolic resin, furan resin, PVA or PVB as a binder; preferably, the binder is 0.5-5 wt% of the total mass of the matrix material and the auxiliary materials; forming a first blank of a desired structure using additive manufacturing techniques; s2: the first green body is immersed in a resin solution.
According to an embodiment of the present invention, in the step S1, the silicon carbide material is one or more of silicon carbide micro powder, chopped silicon carbide fiber, silicon carbide whisker and silicon carbide nanowire; the carbon material is one or more of spheroidal graphite, flake graphite, diamond micropowder, graphene and carbon fiber; preferably silicon carbide micropowder and graphite powder, more preferably silicon carbide micropowder and spheroidal graphite; the mass percentages of the silicon carbide material and the carbon material are 55-100% and 0-45% respectively based on 100% of the total mass of the silicon carbide material and the carbon material.
According to another embodiment of the invention, the additive manufacturing technique in step S1 is stereolithography, powder bed fusion, material extrusion, directional energy deposition, adhesive spraying or thin-film lamination.
According to another embodiment of the present invention, the densification treatment in the step S2 is performed by chemical vapor infiltration or precursor dip cracking.
According to another embodiment of the invention, the first green body has a porosity of 45% to 70%.
According to another embodiment of the present invention, the step S2 further includes: s3: and densifying and/or reaction sintering the first blank after the resin impregnation.
According to another embodiment of the present invention, the densification treatment in the step S3 is performed by chemical vapor infiltration or precursor impregnation pyrolysis; liquid phase siliconizing or gas phase siliconizing is adopted in the reaction sintering; preferably, the gas phase siliconizing is carried out under vacuum or protective atmosphere, the protective atmosphere is one or more of nitrogen, argon and helium, the vacuum degree is 100Pa, the siliconizing temperature is 1550-1800 ℃, the heating rate is 5-15 ℃/min, and the siliconizing time is 0.5-5 h.
According to another embodiment of the invention, the step S2 is repeated after the step S3; preferably, the resin is one or more of epoxy resin, phenolic resin, unsaturated polyester resin, vinyl ester, precursor PDCs polycarbosilane of high-residue Si-based ceramic, polysiloxane and polysilazane resin; more preferably, the green body is immersed in the resin solution, evacuated to 1000pa or less, given a pressure of 0.2-2MPa, and cured at 60-180 ℃.
According to another embodiment of the invention, the porosity of the silicon carbide composite member is 0-70%, the tensile strength is not less than 100Mpa, the flexural strength is not less than 90Mpa, the shear strength is not less than 60Mpa, and the Rockwell hardness is not less than 70HRA.
The invention also provides a silicon carbide composite material component prepared by the method and a pump comprising the component.
The traditional silicon carbide composite material product for preparing large-scale and complex-structure pumps generally adopts a slip casting method, has the defects of complex preparation process, low efficiency and adverse industrialized mass production. The invention adopts a 3D printing method, also called additive manufacturing, and solves the problems of preparation of silicon carbide composite material components for large-scale pumps with complex structures by adopting an improved process, thereby being beneficial to expanding the application field and realizing industrialized mass production.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The preparation method of the silicon carbide composite material component for the 3D printing pump comprises the following steps: s1: selecting a silicon carbide material as a matrix material, optionally selecting a carbon material as an auxiliary material, taking one or more of phenolic resin, furan resin, PVA or PVB as a binder, and forming a first blank with a required structure by adopting an additive manufacturing technology; s2: the first green body is immersed in a resin solution. The blank is immersed in the resin solution to obtain the resin reinforced composite member, so that the fragility of the member is improved, the impact resistance of the member is improved, and the member can bear the impact of solid particles in a slurry pump and is used as a member for the pump. The consumption of the binder is 0.5-5 wt% of the total mass of the matrix material and the auxiliary materials.
In an alternative embodiment, in step S1, the silicon carbide material is one or more of silicon carbide micropowder, chopped silicon carbide fiber, silicon carbide whisker and silicon carbide nanowire; the carbon material is one or more of spheroidal graphite, flake graphite, diamond micropowder, graphene and carbon fiber. Preferably, the matrix material is a fine powder of silicon carbide and graphite powder, more preferably a fine powder of silicon carbide and spheroidal graphite. The mass percentages of the silicon carbide material and the carbon material are respectively 55-100% and 0-45% based on 100% of the total mass of the silicon carbide material and the carbon material.
In step S1, additive manufacturing techniques may be stereolithography, powder bed melting, material extrusion, directional energy deposition, adhesive spraying, or thin-film lamination.
In the step S2, chemical vapor infiltration or precursor dipping and cracking are adopted for densification treatment. The porosity of the first green body obtained by the step is 45% -70%.
In an alternative embodiment, the step S2 may further include: s3: and densifying and/or reaction sintering the first blank after the resin impregnation.
The densification treatment adopts chemical vapor infiltration or precursor dipping and cracking. The reaction sintering adopts liquid phase siliconizing or gas phase siliconizing. The gas phase siliconizing can be carried out under vacuum or protective atmosphere, the protective atmosphere is one or more of nitrogen, argon and helium, the vacuum degree is 100Pa, the siliconizing temperature is 1550 ℃ to 1800 ℃, the heating rate is 5 ℃/min to 15 ℃/min, and the siliconizing time is 0.5h to 5h.
In an alternative embodiment, step S2 is repeated after step S3, i.e. the densified and/or reaction sintered green body is again immersed in the resin solution. The resin solution impregnated in this step may be the same as or different from the resin solution impregnated in the first green body.
The impregnated resin can be one or more of epoxy resin, phenolic resin, unsaturated polyester resin, vinyl ester, precursor PDCs polycarbosilane of high residue Si-based ceramics, polysiloxane and polysilazane resin. After impregnation, curing is performed. The curing conditions are as follows: vacuumizing to below 1000Pa, giving 0.2-2MPa pressure, and solidifying at 60-180deg.C.
According to another embodiment of the invention, the porosity of the silicon carbide composite member is between 0 and 70%. The tensile strength of the obtained silicon carbide composite material component is more than or equal to 100Mpa, the bending strength is more than or equal to 90Mpa, the shearing strength is more than or equal to 60Mpa, and the Rockwell hardness is more than or equal to 70HRA.
The invention also claims a silicon carbide composite material component prepared by the method and a pump comprising the component.
When the silicon carbide composite material member prepared by the method is compounded with the metal framework part to form the pump, one or more layers of resin can be coated on the surface of the silicon carbide composite material member, the silicon carbide composite material member is cured for 3 to 10 hours at the temperature of 60 to 180 ℃, one or more layers of resin is coated on the surface of the metal framework part, and the silicon carbide composite material member is cured for 3 to 10 hours at the temperature of 60 to 180 ℃. And then the component and the metal framework part are combined and assembled into a whole, resin-silicon carbide combined adhesive slurry is filled into a gap between the silicon carbide composite component and the metal framework part, the gap is placed at 60-180 ℃ after filling, and is cured for 6-12 hours to respectively obtain a silicon carbide composite impeller, a front guard plate, a rear guard plate and a pump shell, and the combined impeller, the front guard plate, the rear guard plate and the pump shell are assembled into a complete slurry pump with a metal joint plate, a mechanical seal and a bracket.
Optionally, the resin is one or more of epoxy resin, phenolic resin, unsaturated polyester resin, vinyl ester, precursor PDCs polycarbosilane of high-residue Si-based ceramic, polysiloxane and polysilazane.
The present invention will be further illustrated by the following examples. It should also be understood that the following examples are given by way of illustration only and are not to be construed as limiting the scope of the invention, since various insubstantial modifications and adaptations of the invention to those skilled in the art based on the foregoing disclosure are intended to be within the scope of the invention and the specific process parameters and the like set forth below are merely one example of a suitable range within which one skilled in the art would choose from the description herein without being limited to the specific values set forth below.
Example 1
The silicon carbide powder with the content of 100 percent is taken as a binder, and the dosage of the binder is 3 weight percent of the total mass of the silicon carbide powder. Preparing a component with a complex structure by an SLS (selective laser sintering) 3D printing method, controlling the porosity to be 45%, immersing a silicon carbide blank in a polycarbosilane resin solution, vacuumizing to below 500pa, setting the pressure of 1.6MPa, and curing for 2 hours at a certain temperature of 120 ℃ to obtain the silicon carbide composite material component for the 3D printing pump. A layer of polycarbosilane resin was coated on the surface of the composite member and cured at 120℃for 3 hours, and a layer of resin was coated on the surface of the metal skeleton portion and cured at 120℃for 3 hours. And assembling the silicon carbide composite material component and the metal framework part into a whole, filling resin-silicon carbide combined adhesive slurry into a gap between the silicon carbide composite material component and the metal framework part, placing the mixture at 60 ℃ for curing for 12 hours after filling, respectively obtaining a silicon carbide composite impeller, a front guard plate, a rear guard plate and a pump shell, and assembling the composite impeller, the front guard plate, the rear guard plate and the pump shell with a metal joint plate, a mechanical seal and a bracket into a complete slurry pump.
Example 2
The method comprises the steps of taking 60% of silicon carbide powder, 40% of graphite powder and furan resin as a binder, wherein the dosage of the binder is 1wt% of the total mass of the silicon carbide powder and the graphite powder. Preparing a component with a complex structure by a BJ (binder jet printing) 3D printing method, controlling the porosity to be 50%, immersing a silicon carbide/carbon blank in a phenolic resin solution, vacuumizing to 1000pa, setting the pressure to 0.2MPa, curing for 6 hours at a certain temperature of 120 ℃ to obtain a 3D printed silicon carbide/carbon blank, performing siliconizing reaction sintering on the silicon carbide/carbon blank at 1550 ℃ to obtain a silicon carbide blank with 10% of pores, further immersing the silicon carbide blank in an epoxy resin solution, vacuumizing to less than 500pa, setting the pressure to 1.6MPa, and curing for 2 hours at a certain temperature of 120 ℃ to obtain the silicon carbide composite component for the 3D printing pump. A layer of polycarbosilane resin is coated on the surface of the composite material, and the composite material is cured for 3 hours at 120 ℃, and a layer of polycarbosilane resin is coated on the surface of the metal framework part, and the composite material is cured for 3 hours at 120 ℃. And assembling the silicon carbide composite material component and the metal framework part into a whole, filling the gap between the silicon carbide composite material component and the metal framework part with the polycarbosilane resin-silicon carbide combined adhesive slurry, placing the mixture at 120 ℃ for curing for 6 hours after filling, respectively obtaining a silicon carbide composite impeller, a front guard plate, a rear guard plate and a pump shell, and assembling the composite impeller, the front guard plate, the rear guard plate and the pump shell with a metal joint plate, a mechanical seal and a bracket into a complete slurry pump.
Example 3
The method comprises the steps of mixing 60% of silicon carbide powder, 40% of graphite powder and PVB as a binder, wherein the dosage of the binder is 3% by weight of the total mass of the silicon carbide powder and the graphite powder. Preparing a component with a complex structure by an extrusion molding (DIW) 3D printing method, controlling the porosity to be 50%, immersing a silicon carbide/carbon blank in a phenolic resin solution, vacuumizing to 600pa, setting the pressure to 1.8MPa, curing for 8 hours at a certain temperature of 100 ℃ to obtain a 3D printed silicon carbide/carbon blank, carrying out siliconizing reaction sintering on the silicon carbide/carbon blank at 1600 ℃ to obtain a compact silicon carbide composite material with the porosity of 0%, coating a layer of epoxy resin on the surface of the composite material, curing for 6 hours at 100 ℃, coating a layer of epoxy resin on the surface of a metal framework part, and curing for 6 hours at 100 ℃. And assembling the silicon carbide composite material component and the metal framework part into a whole, filling epoxy resin-silicon carbide combined adhesive slurry into a gap between the silicon carbide composite material component and the metal framework part, placing the gap at 100 ℃ for curing for 12 hours after filling, respectively obtaining a silicon carbide composite impeller, a front guard plate, a rear guard plate and a pump shell, and assembling the composite impeller, the front guard plate, the rear guard plate and the pump shell with a metal joint plate, a mechanical seal and a bracket into a complete slurry pump.
Example 4
The silicon carbide powder with the content of 100 percent is taken as a binder, and the dosage of the binder is 1 weight percent of the total mass of the silicon carbide powder and the graphite powder. The method comprises the steps of preparing a component with a complex structure through a BJ (binder jet printing) 3D printing method, controlling the porosity to be 70%, immersing a silicon carbide blank in a polycarbosilane resin solution, vacuumizing to below 500pa, setting the pressure to be 1.6MPa, and curing for 2 hours at a certain temperature of 120 ℃ to obtain the silicon carbide composite material component for the 3D printing pump. A layer of polycarbosilane resin was coated on the surface of the composite member and cured at 120℃for 3 hours, and a layer of resin was coated on the surface of the metal skeleton portion and cured at 120℃for 3 hours. And assembling the silicon carbide composite material component and the metal framework part into a whole, filling resin-silicon carbide combined adhesive slurry into a gap between the silicon carbide composite material component and the metal framework part, placing the mixture at 60 ℃ for curing for 12 hours after filling, respectively obtaining a silicon carbide composite impeller, a front guard plate, a rear guard plate and a pump shell, and assembling the composite impeller, the front guard plate, the rear guard plate and the pump shell with a metal joint plate, a mechanical seal and a bracket into a complete slurry pump.
Mechanical property tests and corrosion resistance tests were performed on the slurry pump silicon carbide composite material members prepared in examples 1 to 4.
The test results are shown in Table 1
TABLE 1
From the table data, the silicon carbide composite material component for the slurry pump has excellent mechanical property, and the abrasion resistance is far better than that of the A49 duplex stainless white iron material, so that the service life of the slurry pump can be greatly prolonged.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.

Claims (10)

1. A method of making a silicon carbide composite member, comprising:
s1: selecting a silicon carbide material as a matrix material, optionally selecting a carbon material as an auxiliary material, and taking one or more of phenolic resin, furan resin, PVA or PVB as a binder; preferably, the binder is 0.5-5 wt% of the total mass of the matrix material and the auxiliary materials; forming a first blank of a desired structure using additive manufacturing techniques; and
s2: the first green body is immersed in a resin solution.
2. The method of producing a silicon carbide composite material member according to claim 1, wherein in the step S1, the silicon carbide material is one or more of a silicon carbide micro powder, a chopped silicon carbide fiber, a silicon carbide whisker and a silicon carbide nanowire; the carbon material is one or more of spheroidal graphite, flake graphite, diamond micropowder, graphene and carbon fiber; preferably silicon carbide micropowder and graphite powder, more preferably silicon carbide micropowder and spheroidal graphite; the mass percentages of the silicon carbide material and the carbon material are 55-100% and 0-45% respectively based on 100% of the total mass of the silicon carbide material and the carbon material.
3. The method of making a silicon carbide composite material component according to claim 1, wherein the additive manufacturing technique in step S1 is stereolithography, powder bed fusion, material extrusion, directional energy deposition, adhesive spraying, or thin-film lamination.
4. The method of making a silicon carbide composite material member according to claim 1, wherein the first green body has a porosity of 45% to 70%.
5. The method for preparing a silicon carbide composite material member according to claim 1, wherein after the step S2, further comprises:
s3: and densifying and/or reaction sintering the first blank after the resin impregnation.
6. The method of producing a silicon carbide composite material member according to claim 5, wherein the densification treatment in step S3 is performed by chemical vapor infiltration or precursor immersion cracking; liquid phase siliconizing or gas phase siliconizing is adopted in the reaction sintering; preferably, the gas phase siliconizing is carried out under vacuum or protective atmosphere, the protective atmosphere is one or more of nitrogen, argon and helium, the vacuum degree is 100Pa, the siliconizing temperature is 1550-1800 ℃, the heating rate is 5-15 ℃/min, and the siliconizing time is 0.5-5 h.
7. The method of preparing a silicon carbide composite material member according to claim 5, wherein said step S2 is repeated after said step S3;
preferably, the resin is one or more of epoxy resin, phenolic resin, unsaturated polyester resin, vinyl ester, precursor PDCs polycarbosilane of high-residue Si-based ceramic, polysiloxane and polysilazane resin;
more preferably, the green body is immersed in the resin solution, evacuated to 1000pa or less, given a pressure of 0.2-2MPa, and cured at 60-180 ℃.
8. The method of producing a silicon carbide composite material member according to claim 1, wherein the porosity of the silicon carbide composite material member is 0 to 70%, the tensile strength is not less than 100Mpa, the flexural strength is not less than 90Mpa, the shear strength is not less than 60Mpa, and the rockwell hardness is not less than 70HRA.
9. A silicon carbide composite member prepared by the method of any one of claims 1 to 8.
10. A pump comprising the silicon carbide composite member of claim 9.
CN202310564239.0A 2023-05-18 2023-05-18 Silicon carbide composite material member and preparation process method thereof Pending CN116589281A (en)

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