CN113072381B - Method for improving hydration resistance of yttrium oxide ceramic core slurry - Google Patents
Method for improving hydration resistance of yttrium oxide ceramic core slurry Download PDFInfo
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- CN113072381B CN113072381B CN202110410444.2A CN202110410444A CN113072381B CN 113072381 B CN113072381 B CN 113072381B CN 202110410444 A CN202110410444 A CN 202110410444A CN 113072381 B CN113072381 B CN 113072381B
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Abstract
A method for improving hydration resistance of yttria ceramic core slurry comprises the steps of adding yttria powder into a zirconium nitrate precursor solution under the condition of high-speed stirring, and then dropwise adding an ammonia water solution to obtain yttria slurry with the surface coated with zirconium hydroxide; filtering and heating to obtain yttrium oxide powder particles with the surfaces coated with zirconium dioxide, mixing the yttrium oxide powder particles with photocuring resin, and adding a citric acid aqueous solution to obtain the hydration-resistant yttrium oxide ceramic core slurry for photocuring 3D printing. The invention obviously improves the hydration resistance of the yttria powder, keeps the viscosity of the slurry of the ceramic core for photo-curing 3D printing yttria unchanged for a long time, keeps better fluidity and is beneficial to photo-curing 3D printing and forming of the ceramic core.
Description
Technical Field
The invention relates to a technology in the field of ceramic cores, in particular to a method for improving the hydration resistance of a slurry of a photocuring 3D printing yttrium oxide ceramic core.
Background
Hollow castings with complex internal cavity structures, such as hollow air-cooled turbine blades for aircraft engines, gas turbines and other applications, usually adopt ceramic cores to form the internal cavity shapes, but the yttrium oxide ceramic cores prepared by the existing process cannot be separated from molds, so the structural complexity is limited by the molds. In addition, because the yttrium oxide powder is easy to hydrate in water: y is 2 O 3 + physically adsorbed Water → Y 2 O 3 ·H 2 O→Y(OH) 3 →Y 3+ +3OH - That is, water molecules are firstly strongly adsorbed on the surface of yttrium oxide powder particles, and then react with yttrium oxide to generate a yttrium hydroxide layer. Therefore, if the yttria core 3D printing slurry is prepared by using an aqueous light-cured resin solution, the viscosity of the slurry is quickly increased due to the hydration of yttria, so that the core biscuit cannot be timely subjected to 3D printing forming.
Disclosure of Invention
The invention provides a method for improving the hydration resistance of yttria ceramic core slurry aiming at the problem of poor fluidity of the yttria ceramic core slurry caused by hydration of yttria powder in the prior art, which can obviously improve the hydration resistance of yttria powder by coating zirconia on the surfaces of yttria powder particles and adding a surface modifier into the slurry, so that the viscosity of the photo-cured 3D printed yttria ceramic core slurry can be kept unchanged for a long time, better fluidity can be kept, and the photo-cured 3D printed ceramic core slurry is beneficial to photo-cured 3D printing and forming of a ceramic core.
The invention is realized by the following technical scheme:
the invention relates to a method for improving hydration resistance of yttria ceramic core slurry, which comprises the steps of adding yttria powder into zirconium nitrate, zirconium acetate or zirconium oxychloride precursor solution under the condition of high-speed stirring, so that zirconium particles are changed into zirconium hydroxide and coated on the surfaces of electric melting yttria powder particles; then, dropwise adding an ammonia water solution to obtain yttrium oxide slurry with the surface coated with zirconium hydroxide; filtering and heating to obtain yttrium oxide powder particles with the surfaces coated with zirconium dioxide, mixing the yttrium oxide powder particles with light-cured resin, and adding citric acid aqueous solution to obtain the hydration-resistant yttrium oxide ceramic core slurry for light-cured 3D printing.
The mass fraction of the zirconium nitrate, zirconium acetate or zirconium oxychloride precursor solution is 5-20%.
The dosage of the yttrium oxide powder is 10-30% of the mass of the zirconium nitrate, zirconium acetate or zirconium oxychloride precursor solution.
The dosage of the ammonia water solution is 1-3% of the mass of the zirconium nitrate, zirconium acetate or zirconium oxychloride precursor solution.
The heating specifically comprises the following steps: filtering and drying the yttrium oxide slurry coated with zirconium hydroxide on the surface, and then roasting the yttrium oxide slurry in the air at the temperature of 600-1000 ℃ for 2-4h, wherein zirconium hydroxide is decomposed into zirconium dioxide and coated on the surfaces of yttrium oxide powder particles.
The aqueous citric acid solution is preferably added dropwise with stirring.
The preferable mass concentration of the citric acid aqueous solution is 10%.
The yttrium oxide is electric melting yttrium oxide, and the granularity is 325-600 meshes.
The zirconium nitrate, the zirconium acetate and the zirconium oxychloride are all chemically pure.
The preferable mass concentration of the ammonia solution is 10%.
The light-cured resin adopts but is not limited to: any one of water-based urethane acrylate, water-based epoxy acrylate or polyester acrylate.
The photocurable resin preferably contains a photoinitiator, and the photoinitiator is more preferably a radical photoinitiator.
The invention relates to hydration-resistant yttrium oxide ceramic core slurry prepared by the method, which comprises the following components in percentage by mass: 60-90% of yttrium oxide powder coated with zirconium dioxide, 9.5-38.5% of light-cured resin and 0.5-1.5% of citric acid aqueous solution.
Technical effects
The hydration problem of the ceramic slurry for the yttria ceramic core photocuring 3D printing is integrally solved; compared with the prior art, the surface of the electric melting yttrium oxide powder particles is coated with the zirconium oxide by a chemical method, the zirconium oxide has no hydration characteristic, and the coating layer isolates the direct contact of the yttrium oxide and water to a certain extent, so that the hydration resistance of the yttrium oxide powder particles is improved; meanwhile, citric acid is weak acid with carboxyl and hydroxyl, and the groups are easy to adsorb on the surface of the ceramic particles to form a stable chemical structure on the surface of the ceramic particles, so that the reaction tendency of the surface of the yttrium oxide powder particles with water is reduced, and the hydration resistance of the yttrium oxide powder particles is further improved. The effect enables the viscosity of the light-cured 3D printing yttrium oxide ceramic core slurry to be kept unchanged for a long time, and the fluidity is good.
Detailed Description
Example 1
The embodiment comprises the following steps:
step 1) preparing a zirconium nitrate precursor solution: and dissolving 5% by mass of zirconium nitrate in deionized water to prepare a zirconium nitrate precursor solution.
And 2) adding yttrium oxide powder accounting for 10% of the mass fraction of the zirconium nitrate precursor solution into the solution containing the zirconium nitrate precursor under the condition of high-speed stirring, and after all yttrium oxide powder is added, dropwise adding an ammonia water solution accounting for 1% of the mass fraction of the zirconium nitrate precursor solution under the condition of high-speed stirring to change zirconium particles into zirconium hydroxide to coat the zirconium hydroxide on the surfaces of the electric melting yttrium oxide powder particles, thereby obtaining the yttrium oxide slurry with the surfaces coated with the zirconium hydroxide.
And 3) filtering the yttrium oxide slurry with the surface coated with zirconium hydroxide, drying, and roasting in air at 600 ℃ for 4 hours to decompose the zirconium hydroxide into zirconium dioxide coated on the surfaces of yttrium oxide powder particles.
And 4) adding the yttria powder coated with zirconia into the photocuring resin under the condition of stirring, and continuously dropwise adding a citric acid aqueous solution under the condition of stirring, wherein the yttria powder accounts for 90% of the slurry, the water-based polyurethane acrylate accounts for 9.5% of the slurry, and the citric acid aqueous solution accounts for 0.5% of the slurry according to mass fraction, so as to obtain the hydration-resistant yttria ceramic core slurry for photocuring 3D printing.
After the light-cured resin yttrium oxide slurry prepared by uncoated yttrium oxide powder is stirred for 2 hours, the slurry is gelatinized and loses fluidity; the pH value of the yttria ceramic core slurry obtained by the embodiment is 6.5, the viscosity of the yttria ceramic core slurry is 18.4s measured by a No. 4 flow cup, the viscosity is 19.7s measured after the yttria ceramic core slurry is stirred at a low speed of 100 revolutions per minute for 48 hours, the viscosity is increased by only 7.07 percent, no obvious hydrated gel phenomenon is generated visually, the self-leveling property is excellent, and the process requirement of photocuring 3D printing of the yttria ceramic core can be met.
Example 2
The embodiment comprises the following steps:
step 1) preparing zirconium oxychloride precursor solution: and dissolving 12% by mass of zirconium oxychloride in deionized water to prepare a zirconium oxychloride precursor solution.
And 2) adding yttrium oxide powder accounting for 20% of the mass fraction of the zirconium oxychloride zirconium nitrate precursor solution into the solution containing the zirconium nitrate precursor under the condition of high-speed stirring, and after all yttrium oxide powder is added, dropwise adding an ammonia water solution accounting for 2% of the mass fraction of the zirconium nitrate precursor solution under the condition of high-speed stirring to change zirconium particles into zirconium hydroxide to coat the surfaces of the fused yttrium oxide powder particles, thereby obtaining the yttrium oxide slurry with the surfaces coated with the zirconium hydroxide.
And 3) filtering the yttrium oxide slurry with the surface coated with zirconium hydroxide, drying, and roasting in air at 800 ℃ for 3 hours to decompose the zirconium hydroxide into zirconium dioxide coated on the surfaces of yttrium oxide powder particles.
And 4) adding the yttria powder coated with zirconia into the light-cured resin under the condition of stirring, and continuously dropwise adding a citric acid aqueous solution under the condition of stirring, wherein the yttria powder accounts for 75% of the slurry, the water-based epoxy acrylate accounts for 24% of the slurry, and the citric acid aqueous solution accounts for 1% of the slurry according to the mass fraction, so as to obtain the hydration-resistant yttria ceramic core slurry for light-cured 3D printing.
After the light-cured resin yttrium oxide slurry prepared by uncoated yttrium oxide powder is stirred for 2 hours, the slurry is gelatinized and loses fluidity; the pH value of the yttrium oxide ceramic core slurry obtained by the embodiment is 6.3, the viscosity of the yttrium oxide ceramic core slurry is 21.5s measured by a No. 4 flow cup, the viscosity is 22.3s measured after the yttrium oxide ceramic core slurry is stirred at a low speed of 100 revolutions per minute for 48 hours, the viscosity is increased by only 3.72 percent, obvious hydrated gel phenomenon is not generated visually, the self-leveling property is excellent, and the process requirement of photocuring 3D printing of the yttrium oxide ceramic core can be met.
Example 3
The embodiment comprises the following steps:
step 1) preparing a zirconium acetate precursor solution: and dissolving 20% by mass of zirconium nitrate in deionized water to prepare a zirconium nitrate precursor solution.
And 2) adding yttrium oxide powder accounting for 30% of the mass fraction of the zirconium acetate precursor solution into the solution containing the zirconium acetate precursor solution under the condition of high-speed stirring, and after all yttrium oxide powder is added, dropwise adding an ammonia water solution accounting for 3% of the mass fraction of the zirconium acetate precursor solution under the condition of high-speed stirring to change zirconium particles into zirconium hydroxide to coat the zirconium hydroxide on the surfaces of the electric melting yttrium oxide powder particles, thereby obtaining the yttrium oxide slurry with the surfaces coated with the zirconium hydroxide.
And 3) filtering the yttrium oxide slurry with the surface coated with zirconium hydroxide, drying, roasting in the air at 1000 ℃ for 2 hours, and decomposing the zirconium hydroxide into zirconium dioxide coated on the surface of yttrium oxide powder particles.
And 4) adding the yttria powder coated with zirconia into the light-cured resin under the condition of stirring, and continuously dropwise adding a citric acid aqueous solution under the condition of stirring, wherein the yttria powder accounts for 60% of the slurry, the water-based epoxy acrylate accounts for 38.5% of the slurry, and the citric acid aqueous solution accounts for 1.5% of the slurry according to the mass fraction, so as to obtain the hydration-resistant yttria ceramic core slurry for light-cured 3D printing.
After the light-cured resin yttrium oxide slurry prepared by uncoated yttrium oxide powder is stirred for 2 hours, the slurry is gelatinized and loses fluidity; the pH value of the yttrium oxide ceramic core slurry obtained by the embodiment is 5.9, the viscosity of the yttrium oxide ceramic core slurry is measured by a No. 4 flow cup to be 24.4s, the viscosity is measured to be 25.1s after the yttrium oxide ceramic core slurry is stirred at a low speed of 100 revolutions per minute for 48 hours, the viscosity is increased by only 2.87%, no obvious hydrated gel phenomenon is generated by visual observation, the self-leveling property is excellent, and the process requirement of photocuring 3D printing of the yttrium oxide ceramic core can be met.
The embodiment result shows that the technological process is simple, the hydration problem of the photo-cured yttrium oxide ceramic slurry is effectively solved, the requirement of slurry viscosity stability of the yttrium oxide ceramic core in the long-time 3D printing and forming process is met, and the method has good popularization and application values.
The foregoing embodiments may be modified in many different ways by one skilled in the art without departing from the spirit and scope of the invention, which is defined by the appended claims and not by the preceding embodiments, and all embodiments within their scope are intended to be limited by the scope of the invention.
Claims (2)
1. A method for improving hydration resistance of yttria ceramic core slurry is characterized in that electric melting yttria powder is added into zirconium nitrate, zirconium acetate or zirconium oxychloride precursor solution under the condition of high-speed stirring, so that zirconium particles are changed into zirconium hydroxide and coated on the surfaces of the electric melting yttria powder particles; then, dropwise adding an ammonia solution to obtain fused yttrium oxide slurry with the surface coated with zirconium hydroxide; filtering and heating to obtain fused yttrium oxide powder particles with the surfaces coated with zirconium dioxide, mixing the fused yttrium oxide powder particles with photocuring resin, and adding a citric acid aqueous solution to obtain the hydration-resistant yttrium oxide ceramic core slurry for photocuring 3D printing;
the mass fraction of the zirconium nitrate, zirconium acetate or zirconium oxychloride precursor solution is 5-20%;
the using amount of the electric melting yttrium oxide powder is 10-30% of the mass of the zirconium nitrate, zirconium acetate or zirconium oxychloride precursor solution;
the dosage of the ammonia water solution is 1-3% of the mass of the zirconium nitrate, zirconium acetate or zirconium oxychloride precursor solution;
the heating specifically comprises the following steps: filtering and drying the fused yttrium oxide slurry with the surface coated with zirconium hydroxide, and then roasting the fused yttrium oxide slurry in the air at the temperature of 600-1000 ℃ for 2-4h, wherein the zirconium hydroxide is decomposed into zirconium dioxide and is coated on the surfaces of the fused yttrium oxide powder particles;
dropwise adding a citric acid aqueous solution with the mass concentration of 10% under the stirring condition;
the mass concentration of the ammonia water solution is 10 percent;
the light-cured resin adopts the following components: any one of water-based urethane acrylate, water-based epoxy acrylate or polyester acrylate;
the light-cured resin contains a free radical photoinitiator;
the granularity of the electric melting yttrium oxide is 325 meshes to 600 meshes;
the hydration-resistant yttria ceramic core slurry comprises the following components in percentage by mass: the surface of the electric melting yttrium oxide powder coated with zirconium dioxide is 60 to 90 percent, the light curing resin is 9.5 to 38.5 percent, and the citric acid aqueous solution is 0.5 to 1.5 percent.
2. The method of claim 1 wherein the zirconium nitrate, zirconium acetate and zirconium oxychloride are chemically pure.
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| WO2001087798A2 (en) * | 2000-05-19 | 2001-11-22 | The University Of British Columbia | Process for making chemically bonded composite hydroxide ceramics |
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| CN102924062A (en) * | 2012-10-25 | 2013-02-13 | 北京航空航天大学 | Preparation method of calcium-oxide-based ceramic core |
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