CN111039680A - Forming method of silicon-containing ceramic part - Google Patents
Forming method of silicon-containing ceramic part Download PDFInfo
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- CN111039680A CN111039680A CN201911369805.2A CN201911369805A CN111039680A CN 111039680 A CN111039680 A CN 111039680A CN 201911369805 A CN201911369805 A CN 201911369805A CN 111039680 A CN111039680 A CN 111039680A
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Abstract
The invention discloses a forming method of a silicon-containing ceramic part, which is characterized by comprising the following steps of: introducing a group into the silicon-containing ceramic precursor to obtain a photo-curable silicon-containing ceramic precursor; mixing and stirring the photo-curable silicon-containing ceramic precursor, submicron silicon-containing ceramic powder, an element B, a phase solvent, a photoinitiator and a diluent to obtain slurry; forming the slurry to obtain a part blank; and cracking and sintering the part blank to obtain the complex and compact silicon-containing ceramic part. The photo-curable silicon-containing ceramic precursor is used as a binder, the corresponding ceramic powder of submicron level is used as a filling phase, the pollution of impurity elements introduced by other binders can be avoided, the corresponding ceramic phase generated by cracking the precursor can be used for improving the density, and C generated by cracking the precursor can react with oxides on the surface layer of the ceramic powder to improve the sintering driving force.
Description
Technical Field
The invention belongs to the technical field of forming methods of ceramic parts, and relates to a forming method of a silicon-containing ceramic part.
Background
Silicon-containing ceramics such as silicon carbide, silicon nitride and the like have wide application space in the fields of energy heavy industry, chemical engineering, electronic power, aerospace and the like due to a series of excellent performances such as high temperature resistance, high thermal conductivity, strong thermal vibration resistance, good chemical corrosion resistance and the like.
In the traditional forming of ceramic parts such as silicon carbide, silicon nitride and the like, a blank body is generally manufactured through a die, and then the performance of a final finished piece is obtained by four sintering processes of pressureless sintering, hot-pressing sintering, reaction sintering and hot isostatic pressing sintering, so that the cost is high, the period is long, the performance is low, and parts with relatively complex structures cannot be formed; in recent years, silicon-containing ceramic parts such as silicon carbide and silicon nitride have been proposed to be formed by additive manufacturing, but since these are materials with strong covalent bonds and the self-diffusion coefficient in the forming process is very low, the formed parts have the problems of low density, high content of impurity elements, poor use performance and the like, and have a great distance from final engineering application.
Disclosure of Invention
The invention aims to provide a forming method of a silicon-containing ceramic part, which solves the problems of low density and high content of impurity elements in the prior art.
The technical scheme adopted by the invention is that the forming method of the silicon-containing ceramic part is characterized by comprising the following steps:
step 1, introducing a group into a silicon-containing ceramic precursor to obtain a photo-curable silicon-containing ceramic precursor;
step 2, mixing and stirring the photo-curable silicon-containing ceramic precursor, submicron silicon-containing ceramic powder, an element B, a phase solvent, a photoinitiator and a diluent to obtain slurry;
step 3, obtaining a part blank by the slurry through a forming link;
and 4, cracking and sintering the part blank to obtain the complex and compact silicon-containing ceramic part.
The invention is also characterized in that:
the group is one or a combination of a plurality of mercapto, vinyl, acrylate and methacrylate.
Before the photo-curable silicon-containing ceramic precursor is mixed with submicron silicon-containing ceramic powder, the silicon-containing ceramic powder is dried for 2 to 4 hours at the temperature of between 120 and 160 ℃.
The volume ratio of the photo-curable silicon-containing ceramic precursor to the silicon-containing ceramic powder is 1:4-3:2, the mass of the B element is 0.2-0.5% of the mass of the silicon-containing ceramic powder, the mass of the phase solvent is 0.5-1.5% of the mass of the silicon-containing ceramic powder, the mass of the photoinitiator is 0.5-1% of the mass of the photo-curable silicon-containing ceramic precursor, and the amount of the diluent is added according to the viscosity required by the slurry.
The specific process of the step 3 is as follows: and (3) loading the slurry into a photocuring forming device, introducing three-dimensional model information of the ceramic part to be formed, and curing the raw materials layer by layer in a scanning exposure mode under the control of a computer to obtain a complete part blank.
Before cracking the part blank, cleaning, grinding and polishing the part blank.
The specific process for cracking the part blank body comprises the following steps: placing the part blank on a ceramic base plate, then placing the part blank into a heating furnace, raising the temperature to 1000-1400 ℃ at the heating rate of 1-5 ℃/min under the protection of gas, and preserving the temperature for 2-24h to obtain the ceramic component.
The specific process for sintering the part blank comprises the following steps: raising the temperature of the ceramic component to 1600-1800 ℃ at a heating rate of 5-8 ℃/min, preserving the heat for 30-120min, then raising the temperature to 1900-2200 ℃ at a heating rate of 1-3 ℃/min, and preserving the heat for 30-120min to obtain the complex and compact silicon-containing ceramic part.
The invention has the beneficial effects that:
according to the forming method of the silicon-containing ceramic part, the photocurable silicon-containing ceramic precursor is used as the binder, and the submicron corresponding ceramic powder is used as the filling phase, so that the pollution caused by impurity elements introduced by other binders can be avoided; the precursor is used as a binder, so that on one hand, the density of the corresponding ceramic phase can be improved by means of the cracking of the precursor, and on the other hand, C generated by the cracking of the precursor can react with oxides on the surface layer of the ceramic powder to improve the sintering driving force; indirect additive manufacturing is carried out by photocuring reaction, and the precursor and powder are ensured to be formed simultaneously while the preparation of parts with complex shapes is realized; the indirect additive manufacturing is adopted, so that the energy consumption is low and the cost is low; the B is used as a catalyst, so that a solid solution can be formed with the silicon-containing ceramic at high temperature to reduce the interface energy and promote densification; high ceramic yield can be obtained by cracking at 1000-1400 ℃, sintering driving force is improved by sintering at 1900-2200 ℃, and both the high ceramic yield and the high ceramic yield have the effect of improving compactness.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
A method for forming a silicon-containing ceramic part, comprising the steps of:
step 1, introducing a group into a silicon-containing ceramic precursor to obtain a photo-curable silicon-containing ceramic precursor; the group is one or a combination of a plurality of mercapto, vinyl, acrylate and methacrylate.
Step 2, drying the silicon-containing ceramic powder for 2-4 hours at the temperature of 120-160 ℃, and then mixing and stirring the photocurable silicon-containing ceramic precursor, the submicron silicon-containing ceramic powder, the B element, the phase solvent, the photoinitiator and the diluent to obtain slurry;
the volume ratio of the photo-curable silicon-containing ceramic precursor to the silicon-containing ceramic powder is 1:4-3:2, the mass of the B element is 0.2-0.5% of the mass of the silicon-containing ceramic powder, the mass of the phase solvent is 0.5-1.5% of the mass of the silicon-containing ceramic powder, the mass of the photoinitiator is 0.5-1% of the mass of the photo-curable silicon-containing ceramic precursor, and the amount of the diluent is added according to the viscosity required by the slurry.
Preferably, the phase solvent is polyethylene glycol, stearic acid, maleic anhydride, etc., the photoinitiator is benzoin, acetophenone, benzil, etc., and the diluent is multifunctional acrylate, ethoxylated acrylate, propoxylated acrylate, etc.
And 3, filling the slurry into photocuring forming equipment, introducing three-dimensional model information of the ceramic part to be formed, and curing the raw materials layer by layer in a line scanning or surface scanning exposure mode under the control of a computer to obtain a complete part blank.
Organic phase solvents such as alcohol, acetone and the like are used for cleaning uncured materials adhered to the surface of the part blank, the requirement on the surface quality of a final product is high, and the part blank can be cleaned and then subjected to operations such as grinding, polishing and the like.
Step 4, cracking: placing the part blank on a ceramic base plate, then placing the part blank into a heating furnace, raising the temperature to 1000-1400 ℃ at the heating rate of 1-5 ℃/min under the protection of gas, and preserving the temperature for 2-24h to obtain a ceramic component;
and (3) sintering: raising the temperature of the ceramic components to 1600-1800 ℃ at a heating rate of 5-8 ℃/min under the gas protection or vacuum environment, preserving the heat for 30-120min, then raising the temperature to 1900-2200 ℃ at a heating rate of 1-3 ℃/min, preserving the heat for 30-120min, and obtaining the complex and compact silicon-containing ceramic parts.
Through the mode, the forming method of the silicon-containing ceramic part takes the photo-curable silicon-containing ceramic precursor as the binder and the corresponding ceramic powder of submicron level as the filling phase, so that the pollution caused by introducing impurity elements into other binders can be avoided; the precursor is used as a binder, so that on one hand, the density of the corresponding ceramic phase can be improved by means of the cracking of the precursor, and on the other hand, C generated by the cracking of the precursor can react with oxides on the surface layer of the ceramic powder to improve the sintering driving force; indirect additive manufacturing is carried out by photocuring reaction, and the precursor and powder are ensured to be formed simultaneously while the preparation of parts with complex shapes is realized; the indirect additive manufacturing is adopted, so that the energy consumption is low and the cost is low; the B is used as a catalyst, so that a solid solution can be formed with the silicon-containing ceramic at high temperature to reduce the interface energy and promote densification; high ceramic yield can be obtained by cracking at 1000-1400 ℃, sintering driving force is improved by sintering at 1900-2200 ℃, and both the high ceramic yield and the high ceramic yield have the effect of improving compactness.
Example 1
Step 1, introducing vinyl into polycarbosilane to obtain a photocurable silicon carbide precursor
Step 2, drying the silicon carbide powder for 4 hours at 120 ℃, and then mixing and stirring the light-curable silicon carbide precursor, the submicron silicon carbide powder, the element B, the stearic acid, the benzoin dimethyl ether and a proper amount of polyfunctional acrylate to obtain slurry; the volume ratio of the photo-curable silicon carbide precursor to the silicon carbide powder is 3:2, the mass of the B element is 0.2 percent of the mass of the silicon carbide powder, the mass of the stearic acid is 0.5 percent of the mass of the silicon carbide powder, and the mass of the benzoin dimethyl ether is 1 percent of the mass of the photo-curable silicon carbide precursor.
And 3, filling the slurry into photocuring forming equipment, introducing three-dimensional model information of the ceramic part to be formed, and curing the raw materials layer by layer in a surface scanning exposure mode under the control of a computer to obtain a complete part blank. And alcohol is used for cleaning the uncured material adhered to the surface of the part blank.
Step 4, cracking: placing the part blank in a silicon carbide base plate, then placing the part blank in a heating furnace, raising the temperature to 1000 ℃ at the heating rate of 1 ℃/min in the argon environment, and preserving the temperature for 5 hours to obtain a ceramic component;
and (3) sintering: raising the temperature of the ceramic components to 1800 ℃ at a heating rate of 5 ℃/min under an argon environment, preserving the heat for 30min, then raising the temperature to 2200 ℃ at a heating rate of 3 ℃/min, preserving the heat for 30min, and obtaining the complex and compact silicon carbide ceramic part.
Example 2
Step 1, introducing sulfydryl into polycarbosilane to obtain a photocurable silicon carbide precursor;
step 2, drying the silicon carbide powder for 2 hours at the temperature of 150 ℃, and then mixing and stirring the light-curable silicon carbide precursor, the submicron silicon carbide powder, the sintering aid B element, the polyethylene glycol, the Irgacure250 and a proper amount of ethoxylated acrylate to obtain slurry; the volume ratio of the photo-curable silicon carbide precursor to the silicon carbide powder is 1:1, the mass of the B element is 0.5 percent of the mass of the silicon carbide powder, the mass of the polyethylene glycol is 1 percent of the mass of the silicon carbide powder, and the mass of the Irgacure250 is 0.5 percent of the mass of the photo-curable silicon carbide precursor.
And 3, filling the slurry into photocuring forming equipment, introducing three-dimensional model information of the ceramic part to be formed, and curing the raw materials layer by layer in a surface scanning exposure mode under the control of a computer to obtain a complete part blank. And alcohol is used for cleaning the uncured material adhered to the surface of the part blank.
Step 4, cracking: placing the part blank in a silicon carbide base plate, then placing the part blank in a heating furnace, raising the temperature to 1100 ℃ at the heating rate of 5 ℃/min in the argon environment, and preserving the temperature for 3h to obtain a ceramic component and then cooling the ceramic component;
and (3) sintering: raising the temperature of the ceramic components to 1600 ℃ at a heating rate of 5 ℃/min under an argon environment, preserving the heat for 30min, then raising the temperature to 2100 ℃ at a heating rate of 3 ℃/min, and preserving the heat for 120min to obtain the complex and compact silicon carbide ceramic part.
Example 3
Step 1, mixing vinyl silazane resin and multifunctional mercapto resin to obtain a photo-curable silicon nitride precursor;
step 2, drying the silicon nitride powder for 2 hours at 160 ℃, and then mixing and stirring the photo-curable silicon nitride precursor, the submicron silicon nitride powder, the element B, the maleic anhydride, the Irgacure651 and the propoxylated acrylate to obtain slurry; the volume ratio of the photo-curable silicon nitride precursor to the silicon nitride powder is 1:4, the mass of the element B is 0.5 percent of the mass of the silicon nitride powder, the mass of the maleic anhydride is 1.5 percent of the mass of the silicon nitride powder, and the mass of the Irgacure651 is 0.5 percent of the mass of the photo-curable silicon nitride precursor.
And 3, filling the slurry into photocuring forming equipment, introducing three-dimensional model information of the ceramic part to be formed, and curing the raw materials layer by layer in a surface scanning exposure mode under the control of a computer to obtain a complete part blank. And alcohol is used for cleaning the uncured material adhered to the surface of the part blank.
Step 4, cracking: placing the part blank in a silicon nitride backing plate, then placing the part blank in a heating furnace, raising the temperature to 1200 ℃ at the heating rate of 3 ℃/min in a nitrogen environment, and preserving the temperature for 24 hours to obtain a ceramic component and then cooling the ceramic component;
and (3) sintering: under the nitrogen environment, the nitrogen pressure is 1Mpa, the temperature of the ceramic component is increased to 1600 ℃ at the heating rate of 5 ℃/min, the temperature is maintained for 60min, then the temperature is increased to 1900 ℃ at the heating rate of 3 ℃/min, and the temperature is maintained for 60min, so that the complex and compact silicon nitride ceramic part is obtained.
Example 4
Step 1, mixing vinyl silazane resin and multifunctional mercapto resin to obtain a photo-curable silicon nitride precursor;
step 2, drying silicon nitride powder for 2 hours at 150 ℃, and then mixing and stirring the light-curable silicon nitride precursor, submicron silicon nitride powder, element B, stearic acid, benzoin dimethyl ether and a proper amount of polyfunctional acrylate to obtain slurry; the volume ratio of the photo-curable silicon nitride precursor to the silicon nitride powder is 3:2, the mass of the element B is 0.5 percent of the mass of the silicon nitride powder, the mass of the stearic acid is 0.8 percent of the mass of the silicon nitride powder, and the mass of the benzoin dimethyl ether is 0.8 percent of the mass of the photo-curable silicon nitride precursor.
And 3, filling the slurry into photocuring forming equipment, introducing three-dimensional model information of the ceramic part to be formed, and curing the raw materials layer by layer in a surface scanning exposure mode under the control of a computer to obtain a complete part blank. And alcohol is used for cleaning the uncured material adhered to the surface of the part blank.
Step 4, cracking: placing the part blank in a silicon nitride base plate, then placing the part blank in a heating furnace, raising the temperature to 1400 ℃ at the heating rate of 5 ℃/min in the nitrogen environment, and preserving the temperature for 2h to obtain a ceramic component and then cooling the ceramic component;
and (3) sintering: under the nitrogen environment, the nitrogen pressure is 1Mpa, the temperature of the ceramic components is increased to 1800 ℃ at the heating rate of 8 ℃/min, the temperature is maintained for 30min, then the temperature is increased to 1900 ℃ at the heating rate of 1 ℃/min, and the temperature is maintained for 60min, so that the complex and compact silicon nitride ceramic part is obtained.
Claims (8)
1. A method for forming a silicon-containing ceramic part, comprising the steps of:
step 1, introducing a group into a silicon-containing ceramic precursor to obtain a photo-curable silicon-containing ceramic precursor;
step 2, mixing and stirring the photo-curable silicon-containing ceramic precursor, submicron silicon-containing ceramic powder, B element, phase solvent, photoinitiator and diluent to obtain slurry;
step 3, obtaining a part blank by the slurry through a forming link;
and 4, cracking and sintering the part blank to obtain the complex and compact silicon-containing ceramic part.
2. The method of claim 1, wherein the group is one or a combination of mercapto, vinyl, acrylate, and methacrylate.
3. The method as set forth in claim 1, wherein the silicon-containing ceramic powder is dried at 120 ℃ to 160 ℃ for 2 hours before the photocurable silicon-containing ceramic precursor is mixed with the submicron silicon-containing ceramic powder.
4. The method as claimed in claim 1, wherein the volume ratio of the photocurable silicon-containing ceramic precursor to the silicon-containing ceramic powder is 1:4-3:2, the mass of the element B is 0.2-0.5% of the mass of the silicon-containing ceramic powder, the mass of the phase solvent is 0.5-1.5% of the mass of the silicon-containing ceramic powder, and the mass of the photoinitiator is 0.5-1% of the mass of the photocurable silicon-containing ceramic precursor.
5. The method for forming a silicon-containing ceramic part according to claim 1, wherein the specific process of step 3 is as follows: and (3) loading the slurry into a photocuring forming device, introducing three-dimensional model information of the ceramic part to be formed, and curing the raw materials layer by layer in a scanning exposure mode under the control of a computer to obtain a complete part blank.
6. The method as claimed in claim 1, wherein the green body is cleaned, ground and polished before being cracked.
7. The method for forming a silicon-containing ceramic part according to claim 1, wherein the specific process of cracking the part blank is as follows: placing the part blank on a ceramic base plate, then placing the part blank on a heating furnace, raising the temperature to 1000-1400 ℃ at the heating rate of 1-5 ℃/min under the protection of gas, preserving the temperature for 2-24h, and cooling the obtained ceramic component.
8. The method for forming a silicon-containing ceramic part according to claim 1, wherein the sintering of the part blank is carried out by: raising the temperature of the ceramic component to 1600-1800 ℃ at a heating rate of 5-8 ℃/min, preserving the heat for 30-120min, then raising the temperature to 1900-2200 ℃ at a heating rate of 1-3 ℃/min, and preserving the heat for 30-120min to obtain the complex and compact silicon-containing ceramic part.
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