CN112979333A - 3D printing preparation method of potassium titanate whisker reinforced silicon-based ceramic core - Google Patents
3D printing preparation method of potassium titanate whisker reinforced silicon-based ceramic core Download PDFInfo
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Abstract
A3D printing preparation method of a potassium titanate whisker reinforced silicon-based ceramic core comprises the steps of dry mixing quartz glass powder, zirconium silicate powder and potassium titanate whiskers to prepare a ceramic core material, further adding light-cured resin, carrying out ball milling and blending to obtain ceramic core slurry, carrying out 3D printing and layer-by-layer curing to obtain a ceramic core biscuit, placing the ceramic core biscuit in light magnesium oxide powder of a ceramic sagger, sintering in a core sintering furnace to obtain a ceramic core, and finally strengthening by ethyl silicate hydrolysate to obtain the potassium titanate whisker reinforced silicon-based ceramic core. The invention can keep good alkali liquor dissolution performance while obviously improving the high-temperature strength of the silicon-based ceramic core.
Description
Technical Field
The invention relates to a technology in the field of ceramic cores, in particular to a 3D printing preparation method of a silicon-based ceramic core reinforced by potassium titanate whiskers.
Background
The complex hollow structure of the high-temperature alloy turbine blade for the current aeroengine still mostly adopts a silicon-based ceramic core which takes quartz glass as a main raw material to realize forming, the refractoriness of the silicon-based ceramic core is low, the mechanical properties such as high-temperature strength and high-temperature creep resistance are poor, and the complexity of the ceramic core prepared by a hot-pressing injection process is limited by a mold, so that the common hot-pressing injection silicon-based ceramic core can not gradually meet the manufacturing requirement of the high-temperature alloy hollow turbine blade with the complex structure, and the problems of low high-temperature strength and uneven distribution of ceramic fibers in slurry and the core existing in the common silicon-based ceramic core material can not be overcome by the 3D printing technology of ceramics.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a 3D printing preparation method of a silicon-based ceramic core reinforced by potassium titanate whiskers, so that the silicon-based ceramic core can keep good alkali liquor dissolution performance while the high-temperature strength is remarkably improved.
The invention is realized by the following technical scheme:
the invention relates to a 3D printing preparation method of a potassium titanate whisker reinforced silicon-based ceramic core, which comprises the steps of dry mixing quartz glass powder, zirconium silicate powder and potassium titanate whiskers to prepare a ceramic core material, further adding photocuring resin, carrying out ball milling and blending to obtain ceramic core slurry, carrying out 3D printing and layer-by-layer curing to obtain a ceramic core biscuit, placing the ceramic core biscuit in light magnesium oxide powder of a ceramic sagger, sintering in a core sintering furnace to obtain a ceramic core, and finally strengthening by ethyl silicate hydrolysate to obtain the potassium titanate whisker reinforced silicon-based ceramic core.
The core slurry preferably comprises the following components in percentage by weight: 80-94 wt% of quartz glass powder, 2-5 wt% of zirconium silicate powder and 3-15 wt% of potassium titanate whisker.
The quartz glass powder, wherein SiO2The content is more than or equal to 99 wt%, and the particle size distribution is 1-100 mu m.
The zirconium silicate powder, wherein Fe2O3The impurity content is less than or equal to 0.1 wt%, and the particle size distribution is 1-30 mu m.
The potassium titanate whisker has the length of 1-20 microns, the diameter of 0.3-1 micron and the chemical component of K2O·6TiO 2。
The dosage of the light-cured resin accounts for 30-50 wt% of the ceramic core material.
The photo-curing resin is any one of waterborne polyurethane acrylate, waterborne epoxy acrylate or polyester acrylate containing a photoinitiator, the viscosity of the photo-curing resin is less than or equal to 270CPS (30 ℃), and the photo-curing resin can be cured under the irradiation of ultraviolet light to combine ceramic powder together.
The 3D printing specifically comprises the following steps: establishing a 3D model of the ceramic core through a computer, decomposing the model according to layers, decomposing the 3D model into a series of two-dimensional models with the thickness of 25-75 mu m, inputting the established 3D model data into an ultraviolet curing 3D printer, setting a printing program, injecting ceramic core slurry into the 3D printer, and curing, stacking and molding two-dimensional slices layer by layer in an ultraviolet layer-by-layer scanning curing mode to obtain a ceramic core biscuit.
The ceramic core biscuit is preferably soaked in absolute ethyl alcohol to remove redundant uncured resin, the soaking time is 5-10min each time, and the soaking times are 2-4 times.
The ceramic core biscuit is preferably subjected to secondary curing, namely the ceramic core biscuit is put into an ultraviolet curing box to be continuously cured for 1-5 hours.
The sintering comprises the following preferable steps: heating to 200 ℃ and preserving heat for 2h, heating to 500 ℃ and preserving heat for 2h, heating to 1000 ℃ and preserving heat for 2h, then heating to 1200 ℃ and preserving heat for 2h, wherein the heating speed is 30 ℃/h, cooling to room temperature along with the furnace, and then discharging.
The silicon-based ceramic core is preferably subjected to surface powder blowing cleaning after sintering, and is subjected to detection and post-modification by using a core measuring tool.
The strengthening means that: and putting the core into a container filled with ethyl silicate hydrolysate, then putting the container in a negative pressure environment to enable the ethyl silicate hydrolysate to permeate into pores of the core, keeping the soaking time for 2 hours, then putting the core on a frame to be dried for 24 hours, and finally drying the core for 2 hours at 150 ℃ to obtain the potassium titanate whisker reinforced silicon-based ceramic core.
The preferable components and mass percentage of the ethyl silicate hydrolysate are as follows: 34.3 percent of ethyl silicate, 25 percent of absolute ethyl alcohol, 1.5 percent of isopropanol, 13 percent of propylene glycol methyl ether, 25.8 percent of acidic silica sol and 0.4 percent of hydrochloric acid (20 percent of mass concentration) by mixing raw materials and stirring.
The potassium whisker reinforced silicon-based ceramic core prepared by the method is commercially available from all raw materials, and after sintering and strengthening treatment, the porosity of the core is higher than 20%, the surface roughness is lower than 3.2 mu m, the high-temperature bending strength at room temperature and 1500 ℃ is higher than 30MPa, the high-temperature deflection at 1500 ℃ is lower than 1mm, and the core is easy to remove in alkali liquor. Technical effects
The invention integrally solves the problems that the silicon-based ceramic core in the prior art has insufficient high-temperature mechanical property and the forming is limited by a mould. Compared with the prior art, the method has the advantages that the direct forming of the silicon-based ceramic core with the complex structure can be realized without designing and manufacturing a mold for pressing the core, carrying out processes of mold closing, mold stripping and the like, the research and development and manufacturing periods are shortened, the product design freedom is high, errors occur, and the size of a three-dimensional model and the 3D printing process parameters can be directly modified in a computer. The potassium titanate reinforced silicon-based ceramic core has low surface roughness, high size precision, high-temperature strength and excellent high-temperature deformation resistance, so the ceramic core has wide application prospect in the manufacturing field of new generation aeroengine turbine blades, and can be applied to the directional solidification precision casting of the turbine blades of high-performance gas turbines.
Drawings
FIG. 1 is a process flow diagram of the 3D printing preparation of ceramic cores of the present invention;
FIG. 2 is a photograph of the microscopic morphology of potassium titanate whiskers;
FIG. 3 is a microstructure photograph of a ceramic core of the present invention.
Detailed Description
Example 1
As shown in fig. 1, the method for preparing a silicon-based ceramic core reinforced by potassium titanate whiskers according to this embodiment includes the following steps:
1) preparing core slurry: adding 80 wt% of quartz glass powder, 5 wt% of zirconium silicate powder and 15 wt% of potassium titanate whisker shown in figure 2 into a V-shaped mixer, and forcibly stirring and dry-mixing for 5 hours to obtain a ceramic core material; adding water-based polyurethane acrylate accounting for 50 wt% of the ceramic core material into a planetary ball mill, adding the ceramic core material according to the proportion, and carrying out ball milling and blending for 30min to obtain ceramic core slurry.
2) 3D printing of core biscuit: A3D model of the ceramic core is established through a computer, and then the 3D model is decomposed layer by layer through the computer to be decomposed into a series of two-dimensional models with the thickness of 25 mu m. Inputting the established 3D model data into an ultraviolet light curing 3D printer, setting a printing program, injecting the ceramic core slurry obtained in the step 1) into the 3D printer, and curing, stacking and molding the two-dimensional sheets layer by layer in an ultraviolet light layer-by-layer scanning curing mode to obtain a ceramic core biscuit. Soaking the biscuit in anhydrous ethanol for removing excessive uncured resin, wherein the soaking time is 5min each time, and the cleaning times are 4 times.
3) Secondary curing of the core biscuit: putting the ceramic core biscuit obtained in the step 2) into an ultraviolet curing box to be cured for 5 hours continuously.
4) And (3) core sintering: placing the ceramic core biscuit obtained in the step 3) into light magnesium oxide powder of a ceramic sagger, and sintering in a core sintering furnace; the sintering temperature of the core is as follows: heating to 200 ℃ and preserving heat for 2h, heating to 500 ℃ and preserving heat for 2h, heating to 1000 ℃ and preserving heat for 2h, then heating to 1200 ℃ and preserving heat for 2h, wherein the heating speed is 30 ℃/h, cooling to room temperature along with the furnace, and then discharging.
5) And (3) core trimming: and (4) blowing powder on the surface of the sintered ceramic core for cleaning, and then detecting and post-modifying the shape by using a core measuring tool.
6) Core strengthening: putting the core into a container filled with ethyl silicate hydrolysate, placing the container in a negative pressure environment to enable the ethyl silicate hydrolysate to permeate into pores of the core, keeping the soaking time for 2 hours, then placing the core on a rack to be dried for 24 hours, and finally drying the core for 2 hours at 150 ℃ to obtain a final product.
Through detection, the ceramic core prepared by the process has the porosity of 28.98% and the surface roughness (R) shown in figure 3 after sinteringa) 3.12 μm, room temperature bending strength of 39.46MPa, bending strength at 1500 deg.C of 30.13MPa, and high temperature deflection at 1500 deg.C of 0.64 mm; through a decoring test of 8 hours in a decoring kettle with the concentration of the decoring liquid (KOH aqueous solution) of 60 wt%, the pressure of 2.8MPa and the temperature of 360 ℃, the dissolution rate of the ceramic core reaches 100 percent. The detection results show that the ceramic core is suitable for directional solidification molding of the high-temperature alloy hollow blade.
Example 2
The preparation method of the potassium titanate whisker reinforced silicon-based ceramic core comprises the following steps:
1) preparing core slurry: adding 87 wt% of quartz glass powder, 3 wt% of zirconium silicate powder and 10 wt% of potassium titanate whisker into a V-shaped mixer, and forcibly stirring and dry-mixing for 3 hours to obtain a ceramic core material; adding water-based epoxy acrylate accounting for 40 wt% of the ceramic core material into a planetary ball mill, adding the ceramic core material according to the proportion, and carrying out ball milling and blending for 45min to obtain ceramic core slurry.
2) 3D printing of core biscuit: A3D model of the ceramic core is established through a computer, and then the 3D model is decomposed layer by layer through the computer to be decomposed into a series of two-dimensional models with the thickness of 50 mu m. Inputting the established 3D model data into an ultraviolet light curing 3D printer, setting a printing program, injecting the ceramic core slurry obtained in the step 1) into the 3D printer, and curing, stacking and molding the two-dimensional sheets layer by layer in an ultraviolet light layer-by-layer scanning curing mode to obtain a ceramic core biscuit. Soaking the biscuit in anhydrous ethanol for removing excessive uncured resin, wherein the soaking time is 7min each time, and the cleaning times are 3 times.
3) Secondary curing of the core biscuit: putting the ceramic core biscuit obtained in the step 2) into an ultraviolet curing box to be cured for 3 hours continuously.
4) And (3) core sintering: placing the ceramic core biscuit obtained in the step 3) into light magnesium oxide powder of a ceramic sagger, and sintering in a core sintering furnace; the sintering temperature of the core is as follows: heating to 200 ℃ and preserving heat for 2h, heating to 500 ℃ and preserving heat for 2h, heating to 1000 ℃ and preserving heat for 2h, then heating to 1200 ℃ and preserving heat for 2h, wherein the heating speed is 30 ℃/h, cooling to room temperature along with the furnace, and then discharging;
5) and (3) core trimming: and (4) blowing powder on the surface of the sintered ceramic core for cleaning, and then detecting and post-modifying the shape by using a core measuring tool.
6) Core strengthening: putting the core into a container filled with ethyl silicate hydrolysate, placing the container in a negative pressure environment to enable the ethyl silicate hydrolysate to permeate into pores of the core, keeping the soaking time for 2 hours, then placing the core on a rack to be dried for 24 hours, and finally drying the core for 2 hours at 150 ℃ to obtain a final product.
Through detection, the porosity of the ceramic core prepared by the process after sintering is 27.68%, and the surface roughness (R) isa) 2.98 μm, room temperature bending strength 41.45MPa, bending strength 32.37MPa at 1500 deg.C, and high temperature deflection 0.53mm at 1500 deg.C; through a decoring test of 8 hours in a decoring kettle with the concentration of the decoring liquid (KOH aqueous solution) of 60 wt%, the pressure of 2.8MPa and the temperature of 360 ℃, the dissolution rate of the ceramic core reaches 100 percent. The detection results show that the ceramic core is suitable for directional solidification molding of the high-temperature alloy hollow blade.
Example 3
The preparation method of the potassium titanate whisker reinforced silicon-based ceramic core comprises the following steps:
1) preparing core slurry: adding 94 wt% of quartz glass powder, 2 wt% of zirconium silicate powder and 4 wt% of potassium titanate whisker into a V-shaped mixer, and forcibly stirring and dry-mixing for 2 hours to obtain a ceramic core material; adding 30 wt% of waterborne polyurethane acrylate in the ceramic core material into a planetary ball mill, adding the ceramic core material according to the proportion, and carrying out ball milling and blending for 60min to obtain ceramic core slurry.
2) 3D printing of core biscuit: A3D model of the ceramic core is established through a computer, and then the 3D model is decomposed layer by layer through the computer to be decomposed into a series of two-dimensional models with the thickness of 75 mu m. Inputting the established 3D model data into an ultraviolet light curing 3D printer, setting a printing program, injecting the ceramic core slurry obtained in the step 1) into the 3D printer, and curing, stacking and molding the two-dimensional sheets layer by layer in an ultraviolet light layer-by-layer scanning curing mode to obtain a ceramic core biscuit. Soaking the biscuit in anhydrous ethanol for removing excessive uncured resin, wherein the soaking time is 10min each time, and the cleaning times are 2 times.
3) Secondary curing of the core biscuit: putting the ceramic core biscuit obtained in the step 2) into an ultraviolet curing box to be cured for 1 hour.
4) And (3) core sintering: placing the ceramic core biscuit obtained in the step 3) into light magnesium oxide powder of a ceramic sagger, and sintering in a core sintering furnace; the sintering temperature of the core is as follows: heating to 200 ℃ and preserving heat for 2h, heating to 500 ℃ and preserving heat for 2h, heating to 1000 ℃ and preserving heat for 2h, then heating to 1200 ℃ and preserving heat for 2h, wherein the heating speed is 30 ℃/h, cooling to room temperature along with the furnace, and then discharging;
5) and (3) core trimming: and (4) blowing powder on the surface of the sintered ceramic core for cleaning, and then detecting and post-modifying the shape by using a core measuring tool.
6) Core strengthening: putting the core into a container filled with ethyl silicate hydrolysate, placing the container in a negative pressure environment to enable the ethyl silicate hydrolysate to permeate into pores of the core, keeping the soaking time for 2 hours, then placing the core on a rack to be dried for 24 hours, and finally drying the core for 2 hours at 150 ℃ to obtain a final product.
Through detection, the porosity of the ceramic core prepared by the process after sintering is 24.44%, and the surface roughness (R) is detecteda) 2.47 μm, room temperature bending strength 40.28MPa, bending strength 33.16MPa at 1500 deg.C, and bending strength 1500 deg.CThe high-temperature deflection of the steel plate is 0.38 mm; through a decoring test of 8 hours in a decoring kettle with the concentration of the decoring liquid (KOH aqueous solution) of 60 wt%, the pressure of 2.8MPa and the temperature of 360 ℃, the dissolution rate of the ceramic core reaches 100 percent. The detection results show that the ceramic core is suitable for directional solidification molding of the high-temperature alloy hollow blade.
At present, no document report exists on the technology of preparing the ceramic core by using the potassium titanate whisker as a reinforcing phase and combining a 3D printing process. The embodiment result shows that the process is simple, 3D printing preparation of the silicon-based ceramic core with good high-temperature mechanical property and removal property can be directly realized without a die, the period is short, the cost is low, the efficiency is high, and the method is suitable for directional solidification molding of various nickel-based high-temperature alloy hollow turbine blades.
The foregoing embodiments may be modified in many different ways by those skilled in the art without departing from the spirit and scope of the invention, which is defined by the appended claims and all changes that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. A3D printing preparation method of a potassium titanate whisker reinforced silicon-based ceramic core is characterized in that quartz glass powder, zirconium silicate powder and potassium titanate whiskers are dry-mixed to prepare a ceramic core material, then photocuring resin is further added, ball milling and blending are carried out to obtain ceramic core slurry, the ceramic core slurry is solidified layer by layer through 3D printing to obtain a ceramic core biscuit, the ceramic core biscuit is placed in light magnesium oxide powder of a ceramic sagger, a ceramic core is obtained through sintering, and finally the potassium titanate whisker reinforced silicon-based ceramic core is obtained through reinforcement of ethyl silicate hydrolysate;
the core slurry comprises the following components in percentage by weight: 80-94 wt% of quartz glass powder, 2-5 wt% of zirconium silicate powder and 3-15 wt% of potassium titanate whisker;
the dosage of the light-cured resin accounts for 30-50 wt% of the ceramic core material.
2. The potassium titanate whisker reinforced silicon-based of claim 1The 3D printing preparation method of the ceramic core is characterized in that the quartz glass powder is SiO2The content is more than or equal to 99 wt%, and the particle size distribution is 1-100 mu m; the zirconium silicate powder, wherein Fe2O3The impurity content is less than or equal to 0.1 wt%, and the particle size distribution is 1-30 mu m; the potassium titanate whisker has the length of 1-20 microns, the diameter of 0.3-1 micron and the chemical component of K2O·6TiO2。
3. The 3D printing preparation method of the potassium titanate whisker reinforced silicon-based ceramic core according to claim 1, wherein the light-cured resin is any one of water-based polyurethane acrylate, water-based epoxy acrylate or polyester acrylate containing a photoinitiator.
4. The potassium titanate whisker reinforced silicon-based ceramic core 3D printing preparation method according to claim 1, wherein the 3D printing specifically comprises: establishing a 3D model of the ceramic core through a computer, decomposing the model according to layers, decomposing the 3D model into a series of two-dimensional models with the thickness of 25-75 mu m, inputting the established 3D model data into an ultraviolet curing 3D printer, setting a printing program, injecting ceramic core slurry into the 3D printer, and curing, stacking and molding two-dimensional slices layer by layer in an ultraviolet layer-by-layer scanning curing mode to obtain a ceramic core biscuit.
5. The 3D printing preparation method of the potassium titanate whisker reinforced silicon-based ceramic core according to claim 1, wherein the ceramic core biscuit is soaked in absolute ethyl alcohol to remove excessive uncured resin, the soaking time is 5-10min each time, and the soaking times are 2-4 times.
6. The 3D printing preparation method of the potassium titanate whisker reinforced silicon-based ceramic core according to claim 1, 4 or 5, characterized in that the ceramic core biscuit is subjected to secondary curing, namely the ceramic core biscuit is put into an ultraviolet curing box to be continuously cured for 1-5 h.
7. The 3D printing preparation method of the potassium titanate whisker reinforced silicon-based ceramic core according to claim 1, wherein the sintering specifically comprises: heating to 200 ℃ and preserving heat for 2h, heating to 500 ℃ and preserving heat for 2h, heating to 1000 ℃ and preserving heat for 2h, then heating to 1200 ℃ and preserving heat for 2h, wherein the heating speed is 30 ℃/h, cooling to room temperature along with the furnace, and then discharging.
8. The 3D printing preparation method of the potassium titanate whisker reinforced silicon-based ceramic core according to claim 1 or 7, characterized in that the silicon-based ceramic core is subjected to surface powder blowing cleaning after sintering, and is subjected to detection post-modification by a core measuring tool.
9. The 3D printing preparation method of the potassium titanate whisker reinforced silicon-based ceramic core according to claim 1, wherein the strengthening is that: and putting the core into a container filled with ethyl silicate hydrolysate, then putting the container in a negative pressure environment to enable the ethyl silicate hydrolysate to permeate into pores of the core, keeping the soaking time for 2 hours, then putting the core on a frame to be dried for 24 hours, and finally drying the core for 2 hours at 150 ℃ to obtain the potassium titanate whisker reinforced silicon-based ceramic core.
10. The 3D printing preparation method of the potassium titanate whisker reinforced silicon-based ceramic core according to claim 9, wherein the ethyl silicate hydrolysate comprises the following components in percentage by mass: 34.3 percent of ethyl silicate, 25 percent of absolute ethyl alcohol, 1.5 percent of isopropanol, 13 percent of propylene glycol methyl ether, 25.8 percent of acidic silica sol and 0.4 percent of hydrochloric acid with the mass concentration of 20 percent are mixed and stirred to obtain the catalyst.
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Application publication date: 20210618 |