CN109369175B - Method for preparing lanthanum zirconate powder by taking lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials - Google Patents
Method for preparing lanthanum zirconate powder by taking lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials Download PDFInfo
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Abstract
The invention provides a method for preparing lanthanum zirconate powder by taking lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials, which comprises the following steps: preparing lanthanum zirconate precursor powder; respectively adding CeO accounting for 8 wt% of the mass of the lanthanum zirconate precursor powder into the lanthanum zirconate precursor powder2Powders and DyO2Powder; lanthanum zirconate precursor powder and CeO2Powders and DyO2Adding the mixed powder of the powder into a ball milling tank of a high-temperature energy ball mill; according to the ball material ratio of 15: 1-30:1, adding grinding balls into the mixed powder, and sealing the ball milling tank; putting the ball milling tank into a hearth of a high-temperature energy ball mill, heating the hearth to 500 ℃, and preserving heat for 2 hours; vacuumizing the hearth, introducing argon gas for protection, starting a ball mill, raising the temperature of the ball mill to 650-800 ℃, and preserving heat for 12-48 hours; and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the superfine lanthanum zirconate powder with uniform granularity. The method for preparing the lanthanum zirconate powder by taking the lanthanum zirconate precursor powder, the cerium oxide powder and the dysprosium oxide powder as raw materials has the advantages of simple process and low energy consumption, and the obtained lanthanum zirconate powder is uniformly mixed.
Description
Technical Field
The invention relates to the technical field of thermal barrier coating materials, in particular to a method for preparing lanthanum zirconate powder by taking lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials.
Background
With the continuous development of aviation technology and the continuous improvement of requirements on flying speed, flying distance, safety performance and the like, the hot end part of the aero-engine is protected from ablation, corrosion and oxidation of high-temperature gas, the service life of the hot end part is prolonged, and the hot end part becomes the key point of current research. Should at present beThe most widely used Thermal Barrier Coating (TBC) material is Y2O3Partially stabilized ZrO2(YSZ), but when the temperature exceeds 1200 ℃, YSZ is susceptible to phase transformation and sintering, resulting in failure of the coating. And lanthanum zirconate (La)2Zr2O7LZ) has high stability of crystal structure at high temperature, does not undergo phase transition when the temperature is below its melting point (2300 c), and has low sintering rate and thermal conductivity, and is one of the promising high temperature TBC materials. The thermal expansion coefficient is as close as possible to that of the metal substrate, which is the primary reason for selecting the ceramic material of the thermal barrier coating, and the thermal expansion coefficient of the LZ is 8.91-9.1 x 10–6the/K is lower than that of YSZ material, which is the most main factor for restricting the use of LZ on the surface of Ni-based superalloy, but the thermal expansion coefficient of LZ can be obviously increased through ion doping modification.
At present, the method for industrially preparing lanthanum zirconate in more application is a high-temperature solid-phase synthesis method which uses ZrO2And La2O3As a raw material, ZrO is added2And La2O3Drying the powder in a phase box furnace at 1000 deg.C for 1 hr to remove ZrO2And La2O3H absorbed in the powder2O and CO2Then, the dried ZrO is weighed according to the mass ratio of 2: 12And La2O3Putting the powder into a ball milling tank, and adding ZrO twice the total mass of the mixed powder2Grinding the balls, adding ultrapure water which is twice the total mass of the mixed powder into a ball milling tank, mixing the materials and carrying out ball milling for 48 hours. And then, the slurry after ball milling is sieved by a 200-mesh sieve and dried, and finally, the mixture is put into a crucible and placed into a box-type furnace, and is calcined and synthesized at the temperature of 1200-1600 ℃, and the heat preservation time is 12 hours. The lanthanum zirconate is synthesized by calcining at the high temperature of 1200-1600 ℃, so that the method has the advantages of complex production process, high energy consumption and high cost, and the powder obtained by the method has the problems of nonuniform micro-mixing, composition segregation, nonuniform micro-structure, serious agglomeration and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing lanthanum zirconate powder by taking lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials, which has the advantages of simple process, low energy consumption and uniform mixing of the obtained powder.
In order to solve the technical problems, the invention provides a method for preparing lanthanum zirconate powder by taking lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials, which comprises the following steps:
preparing lanthanum zirconate precursor powder;
respectively adding CeO accounting for 8 wt% of the mass of the lanthanum zirconate precursor powder into the lanthanum zirconate precursor powder2Powders and DyO2Powder;
lanthanum zirconate precursor powder and CeO2Powders and DyO2Adding the mixed powder of the powder into a ball milling tank of a high-temperature energy ball mill;
according to the ball material ratio of 15: 1-30:1 oriented lanthanum zirconate precursor powder and CeO2Powders and DyO2Adding grinding balls into the mixed powder of the powder, and sealing the ball milling tank;
putting the ball milling tank into a hearth of a high-temperature energy ball mill, heating the hearth to 500 ℃, and preserving heat for 2 hours;
vacuumizing the hearth, introducing argon gas for protection, starting a ball mill, raising the temperature of the ball mill to 650-800 ℃, and preserving heat for 12-48 hours;
and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the superfine lanthanum zirconate powder with uniform granularity.
Further, the preparation method of the lanthanum zirconate precursor powder comprises the following steps:
la2O3Dissolving in hydrochloric acid to obtain La3+La with concentration of 0.5mol/L3+Solution, ZrOCl2·8H2Dissolving O in water to obtain Zr4+Zr concentration of 0.5mol/L4+A solution;
la3+Solution and Zr4+Mixing the solutions, dropwise adding ammonia water into the mixed solution to generate a precipitate, heating and stirring the solid-liquid system at the water bath temperature of 60 ℃, and dropwise adding ammonia water to ensure that the pH value of the system is constant to 10;
heating and stirring for 25-40min, carrying out suction filtration on a solid-liquid system, and washing the precipitate until the pH value of the washing liquid is 7;
drying the precipitate at the temperature of 110-130 ℃ for 11-13h, then grinding and sieving by a 200-mesh sieve to obtain the lanthanum zirconate precursor powder.
The method for preparing the lanthanum zirconate powder by taking the lanthanum zirconate precursor powder, the cerium oxide powder and the dysprosium oxide powder as raw materials adopts a method of heating, calcining and ball-milling in the same high-temperature reaction furnace, because the ball-milling environment temperature is high, the lanthanum zirconate precursor powder can obtain enough energy in a short time, is rapidly decomposed and accumulated, and the ball-milling force and the external temperature rise of a system are simultaneously carried out, so that the absorption of the lanthanum zirconate precursor particles on the energy are promoted, the temperature of the reaction system can rapidly reach and exceed the critical temperature of the synthesized lanthanum zirconate, the reaction rate of the system is accelerated, the lanthanum zirconate powder with small granularity can be obtained in a short time, the operation steps are simplified, the reaction time is saved, the energy loss is reduced, and the cost is saved. And the proper ball milling refines the crystal grains and increases the specific surface area, thereby improving the kinetic condition, leading the conventional high-temperature solid-phase synthesis method to carry out more complete reaction under the high-temperature condition of 1200-1600 ℃, and being realized at lower temperature of 650-800 ℃, compared with the conventional high-temperature solid-phase synthesis method, the temperature is reduced by 450-850 ℃, thereby further reducing the energy consumption and saving the cost. Due to the existence of the ball milling, the occurrence of agglomeration is reduced, the powder is further refined and dispersed more uniformly, reactants and products are continuously refined, and the lanthanum zirconate powder which has good dispersibility, uniform micro mixing, large grain size, small grain size, uniform microstructure and no agglomeration is obtained. Meanwhile, the lanthanum zirconate powder prepared by the invention has higher thermal expansion coefficient and Y2O3Partially stabilized ZrO2The thermal expansion coefficient of the material (YSZ) is very similar, namely the thermal expansion coefficient of the material is similar to that of the Ni-based high-temperature alloy material, and the material is suitable for being used on the surface of the Ni-based high-temperature alloy.
Drawings
Fig. 1 is a flow chart of a method for preparing lanthanum zirconate powder by using lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials according to an embodiment of the invention;
fig. 2 is an X-ray diffraction pattern of lanthanum zirconate powder prepared by a method for preparing lanthanum zirconate powder by using lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials according to an embodiment of the present invention;
fig. 3 is a particle size diagram of lanthanum zirconate powder prepared by the method for preparing lanthanum zirconate powder by using lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials according to the embodiment of the invention.
Detailed Description
Referring to fig. 1, the method for preparing lanthanum zirconate powder by using lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials, provided by the embodiment of the invention, comprises the following steps:
step 1, preparing lanthanum zirconate precursor powder: la2O3Dissolving in hydrochloric acid to obtain La3+La with concentration of 0.5mol/L3+Solution, ZrOCl2·8H2Dissolving O in water to obtain Zr4+Zr concentration of 0.5mol/L4+A solution; then La is added3+Solution and Zr4+Mixing the solution and stirring in a constant-temperature magnetic stirrer, dropwise adding a precipitant such as ammonia water into the mixed solution to immediately generate white, light purple or light yellow flocculent precipitate, heating and stirring the solid-liquid system after the precipitate is generated at the water bath temperature of 60 ℃, and dropwise adding ammonia water to ensure that the pH value of the system is constant to 10; after 25-40min, carrying out suction filtration on the solid-liquid system, and repeatedly washing the precipitate with distilled water continuously until the pH value of the washing liquid is 7; and finally, putting the obtained precipitation filter cake into a culture dish, drying at the temperature of 110-130 ℃ for 11-13h, grinding, and sieving by a 200-mesh sieve to obtain the lanthanum zirconate precursor powder. The chemical reactions that occur in this process are as follows:
step 3, lanthanum zirconate precursor powder and CeO2Powders and DyO2Adding the mixed powder of the powder into a ball milling tank of a high-temperature energy ball mill;
step 5, putting the ball milling tank into a hearth of a high-temperature energy ball mill, heating the hearth to 500 ℃, and preserving heat for 2 hours;
and 7, closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the superfine lanthanum zirconate powder with uniform granularity.
Referring to fig. 2 and 3, in the method for preparing lanthanum zirconate powder by using lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials according to the embodiment of the invention, the prepared lanthanum zirconate powder has the advantages of good dispersibility, uniform micro-mixing, large grain size, small grain size, uniform microstructure and no agglomeration, and the prepared lanthanum zirconate powder has a high thermal expansion coefficient and is combined with Y2O3Partially stabilized ZrO2The thermal expansion coefficient of the material (YSZ) is very similar, and the material is suitable for being used on the surface of the Ni-based high-temperature alloy material. Meanwhile, the superfine La prepared by the invention2Zr2O7In the powder, Ce is solid-dissolved in a lanthanum zirconate crystal lattice to replace Zr atom positions, and the doping amount of Dy and Ce does not change the crystal structure of the lanthanum zirconate within a certain range.
The method for preparing lanthanum zirconate powder using lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials according to the present invention will be specifically described below with reference to specific examples.
Example 1
Superfine La2Zr2O7The preparation process of the powder comprises the following steps:
(1) la2O3Dissolved in hydrochloric acid, ZrOCl2·8H2Dissolving O in water to prepare cations La respectively3+And Zr4+And (3) mixing and stirring the solution with the concentration of 0.5mol/L in a constant-temperature magnetic stirrer, dropwise adding ammonia water into the mixed solution to react to generate flocculent precipitate, then adjusting the temperature of the water bath to 60 ℃, continuously stirring, and simultaneously dropwise adding ammonia water to ensure that the pH value of the system is constant to 10. And continuously stirring for 30min, performing suction filtration, repeatedly washing and precipitating by using distilled water until the pH value of a washing liquid is 7, finally putting a filter cake obtained by suction filtration into a culture dish, drying at 120 ℃ for 12h, and grinding and sieving by using a 200-mesh sieve to obtain lanthanum zirconate precursor powder.
(2) Uniformly mixing 100g of lanthanum zirconate precursor powder, 8g of cerium oxide powder and 8g of dysprosium oxide powder to obtain a reactant;
(3) putting the powder into a stainless steel ball milling tank, adding a stainless steel ball, wherein the ball-material ratio is 15: 1;
(4) putting the ball milling tank into a high-temperature energy ball mill;
(5) heating the ball mill to 500 ℃, and preserving heat for 2 hours;
(6) vacuumizing the ball mill and introducing argon as protective gas;
(7) starting the ball mill, continuously rotating, simultaneously heating the hearth to 800 ℃, and preserving heat for 12 hours;
(8) and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the lanthanum zirconate powder with uniform granularity.
Example 2
Superfine La2Zr2O7The preparation process of the powder comprises the following steps:
(1) la2O3Dissolved in hydrochloric acid, ZrOCl2·8H2Dissolving O in water to prepare cations La respectively3+And Zr4+The solution with the concentration of 0.5mol/L is mixed and stirred in a constant temperature magnetic stirrerAnd dropwise adding ammonia water into the mixed solution to react to generate flocculent precipitate, then adjusting the temperature of the water bath to 60 ℃, continuously stirring, and simultaneously dropwise adding ammonia water to ensure that the pH value of the system is constant to 10. And continuously stirring for 25min, performing suction filtration, repeatedly washing and precipitating by using distilled water until the pH value of a washing liquid is 7, finally putting a filter cake obtained by suction filtration into a culture dish, drying at 110 ℃ for 13h, grinding and sieving by using a 200-mesh sieve to obtain lanthanum zirconate precursor powder.
(2) Uniformly mixing 100g of lanthanum zirconate precursor powder, 8g of cerium oxide powder and 8g of dysprosium oxide powder to obtain a reactant;
(3) putting the powder into a stainless steel ball milling tank, adding zirconia balls, wherein the ball-to-material ratio is 25: 1;
(4) putting the ball milling tank into a high-temperature energy ball mill;
(5) heating the ball mill to 500 ℃, and preserving heat for 2 hours;
(6) vacuumizing the ball mill and introducing argon as protective gas;
(7) starting the ball mill, continuously rotating, simultaneously heating the hearth to 750 ℃, and preserving heat for 24 hours;
(8) and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the lanthanum zirconate powder with uniform granularity.
Example 3
Superfine La2Zr2O7The preparation process of the powder comprises the following steps:
(1) la2O3Dissolved in hydrochloric acid, ZrOCl2·8H2Dissolving O in water to prepare cations La respectively3+And Zr4+And (3) mixing and stirring the solution with the concentration of 0.5mol/L in a constant-temperature magnetic stirrer, dropwise adding ammonia water into the mixed solution to react to generate flocculent precipitate, then adjusting the temperature of the water bath to 60 ℃, continuously stirring, and simultaneously dropwise adding ammonia water to ensure that the pH value of the system is constant to 10. And continuously stirring for 40min, performing suction filtration, repeatedly washing and precipitating by using distilled water until the pH value of a washing liquid is 7, finally putting a filter cake obtained by suction filtration into a culture dish, drying at 130 ℃ for 11h, and grinding and sieving by using a 200-mesh sieve to obtain lanthanum zirconate precursor powder.
(2) Uniformly mixing 100g of lanthanum zirconate precursor powder, 8g of cerium oxide powder and 8g of dysprosium oxide powder to obtain a reactant;
(3) putting the powder into a stainless steel ball milling tank, adding a stainless steel ball, wherein the ball-material ratio is 30: 1;
(4) putting the ball milling tank into a high-temperature energy ball mill;
(5) heating the ball mill to 500 ℃, and preserving heat for 2 hours;
(6) vacuumizing the ball mill and introducing argon as protective gas;
(7) starting the ball mill, continuously rotating, simultaneously heating the hearth to 650 ℃, and preserving heat for 48 hours;
(8) and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the lanthanum zirconate powder with uniform granularity.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (1)
1. A method for preparing lanthanum zirconate powder by taking lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials is characterized by comprising the following steps of:
preparing lanthanum zirconate precursor powder;
respectively adding CeO accounting for 8 wt% of the mass of the lanthanum zirconate precursor powder into the lanthanum zirconate precursor powder2Powders and DyO2Powder;
lanthanum zirconate precursor powder and CeO2Powders and DyO2Adding the mixed powder of the powder into a ball milling tank of a high-temperature energy ball mill;
according to the ball material ratio of 15: 1-30:1 oriented lanthanum zirconate precursor powder and CeO2Powders and DyO2Adding grinding balls into the mixed powder of the powder, and sealing the ball milling tank;
putting the ball milling tank into a hearth of a high-temperature energy ball mill, heating the hearth to 500 ℃, and preserving heat for 2 hours;
vacuumizing the hearth, introducing argon gas for protection, starting a ball mill, raising the temperature of the ball mill to 650-800 ℃, and preserving heat for 12-48 hours;
closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain superfine lanthanum zirconate powder with uniform granularity;
the thermal expansion coefficient and Y of the lanthanum zirconate powder2O3Partially stabilized ZrO2The thermal expansion coefficients of the materials are similar, and the material is suitable for being used on the surface of a Ni-based high-temperature alloy material;
the preparation method of the lanthanum zirconate precursor powder comprises the following steps:
la2O3Dissolving in hydrochloric acid to obtain La3+La with concentration of 0.5mol/L3+Solution, ZrOCl2·8H2Dissolving O in water to obtain Zr4+Zr concentration of 0.5mol/L4+A solution;
la3+Solution and Zr4+Mixing the solutions, dropwise adding ammonia water into the mixed solution to generate a precipitate, heating and stirring the solid-liquid system at the water bath temperature of 60 ℃, and dropwise adding ammonia water to ensure that the pH value of the system is constant to 10;
heating and stirring for 25-40min, carrying out suction filtration on a solid-liquid system, and washing the precipitate until the pH value of the washing liquid is 7;
drying the precipitate at the temperature of 110-130 ℃ for 11-13h, then grinding and sieving by a 200-mesh sieve to obtain the lanthanum zirconate precursor powder.
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Citations (2)
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|---|---|---|---|---|
| CN101003024A (en) * | 2006-09-19 | 2007-07-25 | 东北大学 | High temperature energy ball grinder |
| CN101200375A (en) * | 2007-11-16 | 2008-06-18 | 北京矿冶研究总院 | Preparation method of nano zirconium-containing series thermal barrier coating material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003024A (en) * | 2006-09-19 | 2007-07-25 | 东北大学 | High temperature energy ball grinder |
| CN101200375A (en) * | 2007-11-16 | 2008-06-18 | 北京矿冶研究总院 | Preparation method of nano zirconium-containing series thermal barrier coating material |
Non-Patent Citations (2)
| Title |
|---|
| Coprecipitation synthesis and thermal conductivity of La2Zr2O7;Hongfei Chen et al.;《Journal of Alloys and Compounds》;20090304;第480卷(第2期);第844页第2、3段，第846页图5和6 * |
| 稀土Dy和Ce共掺杂La2Zr2O7新型热障涂层用陶瓷材料;周宏明等;《无机材料学报》;20080531;第23卷(第3期);第568页左栏第3段，右栏第2段，第571页右栏第5段 * |
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