CN111153434A - Preparation method of lanthanum zirconate spherical powder for thermal spraying - Google Patents
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Abstract
The invention discloses a preparation method of lanthanum zirconate spherical powder for thermal spraying, which comprises the following steps: mixing La with the molar ratio of 1:22O3And ZrO2Uniformly mixing the mixture and a molten salt medium through wet ball milling, drying the mixture, heating to 900-1200 ℃, preserving heat for 4-10 hours, and cooling to room temperature; washing the reaction product with water to remove residual molten salt medium, adding a binder and deionized water to obtain slurry, and granulating the slurry by using spray drying equipment to obtain spherical powder; calcining the prepared spherical powder at high temperature to remove the binder in the spherical powder andthe spherical powder is densified to obtain the lanthanum zirconate spherical powder for thermal spraying. The invention provides a liquid phase environment by using the molten salt as a reaction medium, reduces the reaction temperature and avoids the growth of particles; the method adopts the oxide as the raw material, has higher conversion efficiency and production efficiency, can recycle the molten salt, has low synthesis cost, short time and simple operation, and is suitable for mass production.
Description
Technical Field
The invention belongs to the technical field of functional material preparation, and particularly relates to a preparation method of lanthanum zirconate spherical powder for preparing a thermal barrier coating by an explosion spraying process.
Background
As aircraft engines move toward high thrust-to-weight ratios, the inlet temperature of turbine engines continues to increase. The thermal barrier coating is a thermal protection technology for coating a high-temperature-resistant, corrosion-resistant and high-heat-insulation ceramic material on the surface of a base alloy so as to improve the high-temperature oxidation corrosion resistance of the base alloy and reduce the working temperature of the surface of the alloy, and has a vital effect on protecting a hot-end part of an engine. At present, the yttrium-stabilized zirconia (YSZ) which has the best comprehensive performance and is most widely applied is a thermal barrier coating material part, and the phase change and sintering can occur at the temperature of more than 1200 ℃, so that the application of the yttrium-stabilized zirconia at higher temperature is limited.
Lanthanum zirconate has excellent performances such as low thermal conductivity, sintering resistance, phase stability and the like, and is one of materials expected to replace (YSZ) at higher use temperature. In the process of preparing the thermal barrier coating by the thermal spraying process, the grain size distribution and the shape of the lanthanum zirconate powder can influence the bonding strength, the porosity, the heat-insulating property and the thermal shock resistance of the prepared coating. And lanthanum zirconate particles with undersize particle sizes have poor flowability and dispersibility, are easy to accumulate in a powder feeder in the powder feeding process, and greatly reduce the deposition efficiency of spraying, so that the lanthanum zirconate aggregates with the particle sizes of 20-200 mu m are usually obtained by granulation and used for explosion spraying.
In the related technology, the preparation of the lanthanum zirconate spherical powder adopts a coprecipitation method to synthesize lanthanum zirconate nano powder, the lanthanum zirconate spherical powder meeting the spraying requirement is obtained by a spray granulation method, although the process flow can be shortened by carrying out filter pressing on precipitates and then carrying out size mixing and direct granulation, the consumption time of the precipitation and aging process is still long (more than 12 h-24 h), the efficiency is not high, and the cost is high by taking zirconium salt and lanthanum salt as raw materials.
Chinese patent application 2018100363357 discloses a method for preparing thermal spraying spherical lanthanum zirconate powder, which comprises the following steps: 1) mixing a lanthanum salt solution and a zirconium salt solution according to the proportion of 1:1, mixing and stirring uniformly; 2) preparing a precipitate by using ammonia water or ammonium oxalate as a precipitating agent; 3) carrying out ceramic membrane and filter pressing treatment on the precipitate; 4) directly granulating after nitric acid slurry mixing; 5) and (4) carrying out heat treatment on the granulated powder to obtain spherical lanthanum zirconate powder with a single pyrochlore crystal phase. Compared with the granulation method in the related technology, the method shortens the process flow, the obtained spherical powder has high sphericity, good fluidity and high density, reaches the performance index of secondary plasma granulation powder, reduces the cost, and is suitable for large-scale industrial production. The method is synthesized by directly mixing and granulating the precipitate and then calcining, and the final product can be obtained only by one-time high-temperature treatment, thereby shortening the process flow and reducing the cost compared with the traditional coprecipitation method. However, the synthesis process of the powder takes zirconium salt and lanthanum salt as raw materials, the cost is high, the precipitation and aging process consumes long time, and the method has the problem that the excessive growth among particles is difficult to control.
Disclosure of Invention
The invention provides a preparation method of lanthanum zirconate spherical powder, which is used for an explosive spraying process and has different diameters and is obtained by adopting a molten salt-assisted solid phase method for synthesis and spray granulation.
According to the invention, low-cost metal oxide is used as a raw material, cheap potassium and sodium salt which can be recycled are used as reaction media, and compared with a coprecipitation method, the method does not need long-time processes of titration, stirring, aging and the like, and solves the problems of long production cycle and overhigh cost of metal salts of the coprecipitation method; compared with the traditional solid phase method, the fused salt is used as a reaction medium to provide a liquid phase mass transfer environment, so that the problems of high synthesis temperature and large particles in the solid phase method are solved, and the prepared powder is more uniform in shape.
The purpose of the invention is realized by the following technical scheme:
a preparation method of lanthanum zirconate spherical powder for thermal spraying comprises the following steps:
1) mixing La with the molar ratio of 1:22O3And ZrO2Mixing with molten salt medium by wet ball milling, drying the mixture, and heating to 900 deg.CKeeping the temperature at 1200 ℃ for 4-10 hours, and cooling to room temperature; the molten salt medium is sodium chloride and potassium chloride with the mass ratio of 1: 0.8-1: 1.25;
2) washing the reaction product with water to remove residual molten salt medium, adding a binder and deionized water to obtain slurry, and granulating the slurry by using spray drying equipment to obtain spherical powder;
3) and calcining the prepared spherical powder at high temperature to remove the binder and densify the spherical powder to obtain the lanthanum zirconate spherical powder for thermal spraying.
To further achieve the object of the present invention, preferably, in step 1), the La is2O3And ZrO2The mass ratio of the total mass to the molten salt medium is 1: 0.5-1: 1.
Preferably, in the step 1), the wet ball milling refers to adding the mixture, zirconia balls and absolute ethyl alcohol into a ball milling tank according to a mass ratio of 1:2:1.578, and ball milling is carried out for 2-6 hours at a speed of 300-600 r/min; the mixture is La2O3、ZrO2With a molten salt medium.
Preferably, in the step 1), the temperature is raised to 900-1200 ℃ at a speed of 1-10 ℃/min.
Preferably, in step 1), said La2O3Has a purity of 99% or more, ZrO2The purity of (A) is more than 99.8%, and the particle size is 40-500 nm.
Preferably, in the step 2), the washing is to add the reaction product into deionized water in proportion, stir for 5-15 minutes, and perform suction filtration; repeating the steps of adding deionized water into the obtained filter cake according to the proportion, stirring and filtering for 3-6 times; the step of adding deionized water in proportion refers to adding 150-250 g of reaction product into every 500ml of deionized water.
Preferably, in step 2), the binder is a PVA solution with a mass concentration of 10%.
Preferably, in the step 2), the solid content of the slurry is 50-70% by mass percentage.
Preferably, in the step 3), the high-temperature calcination treatment refers to heating to 1300-1500 ℃ at a speed of 1-3 ℃/min, preserving heat for 2-5 h, and then cooling along with a furnace.
Preferably, in the step 3), the grain size of the lanthanum zirconate spherical powder for thermal spraying is 100-500 nm, and the grain size distribution is 20-100 μm.
Compared with the prior art, the invention has the beneficial effects that: molten salt is used as a reaction medium to provide a liquid phase environment, so that the reaction temperature is reduced, and the growth of particles is avoided; the method adopts the oxide as the raw material, has higher conversion efficiency and production efficiency, can recycle the molten salt, has low synthesis cost, short time and simple operation, and is suitable for mass production.
Drawings
FIG. 1 is a comparison of the XRD spectrum of the powder prepared in example 1 of the present invention and lanthanum zirconate standard card 07-0444.
FIG. 2 is a scanning electron micrograph of the powder prepared in example 1 of the present invention magnified 100 times.
FIG. 3 is a scanning electron micrograph of the powder prepared in example 1 of the present invention magnified 3000 times.
Detailed Description
For a better understanding of the present invention, the present invention is further described below with reference to the accompanying drawings and examples, but the embodiments of the present invention are not limited to the examples.
Example 1
1) Lanthanum oxide and zirconium oxide were used as starting materials, with lanthanum oxide purity of 99.8 wt.% and zirconium oxide purity of 99.99 wt.%. 34.16g of lanthanum oxide, 25.84g of zirconium oxide, 33.28g of potassium chloride and 26.72g of sodium chloride are weighed by a balance, added into a ball milling tank together with 240g of zirconium oxide balls and 240mL of ethanol, and ball milled for 2 hours at 480 r/min. Taking out, drying, placing into a muffle furnace, heating to 1200 ℃ at a speed of 5 ℃/min, preserving heat for 4h, and cooling to room temperature along with the furnace.
2) Washing with deionized water and performing suction filtration, repeating the washing and the suction filtration for 3 times, adding 25g of 10 wt.% PVA solution into a filter cake, uniformly stirring to obtain slurry, and granulating by using airflow type spray drying equipment, wherein the inlet temperature is 240 ℃ and the outlet temperature is 120 ℃;
3) and (3) putting the powder obtained after spray granulation into a muffle furnace, heating to 1300 ℃ at a speed of 3 ℃/min, preserving heat for 3h, and cooling along with the furnace to obtain the lanthanum zirconate spherical powder for thermal spraying.
Fig. 1 is an XRD spectrum of example 1, and it can be seen that the powder synthesized in this example 1 is single-phase pyrochlore-structured lanthanum zirconate and contains no other hetero-phase. Fig. 2 and 3 are scanning electron microscope pictures of the obtained spherical powder with different magnifications, which show that the particle size of the spherical powder is 20-100 μm, most of the particles are intensively distributed between 40-60 μm and are aggregates formed by micron-sized small particles, and the particles do not grow excessively and are uniform in size. The powder has high sphericity, particle size distribution of 20-100 μm and fluidity of 44.80/50g, and can meet the requirements of various thermal spraying.
Some Yttrium Stabilized Zirconia (YSZ) has limited its use at higher temperatures due to phase transformation and sintering above 1200 ℃. Lanthanum zirconate has excellent performances of low thermal conductivity, sintering resistance, phase stability and the like, and can have better thermal insulation and thermal shock resistance and longer service life than YSZ when used as a thermal barrier coating at the temperature of more than 1200 ℃. The method adopts the molten salt as a reaction medium to provide a liquid phase mass transfer environment, reduces the temperature by about 400-600 ℃ compared with the traditional solid phase method, can recycle the molten salt, and has almost negligible cost compared with the raw material. Solves the problems of high synthesis temperature (above 1600 ℃), long time, uneven and large particles and the like of a solid phase method, and ensures that the prepared powder has more uniform appearance.
Example 2
1) Lanthanum oxide and zirconium oxide were used as starting materials, with lanthanum oxide purity of 99.8 wt.% and zirconium oxide purity of 99.99 wt.%. 34.16g of lanthanum oxide, 25.84g of zirconium oxide, 33.28g of potassium chloride and 26.72g of sodium chloride are weighed by a balance, added into a ball milling tank together with 240g of zirconium oxide balls and 240mL of ethanol, and ball milled for 2 hours at 480 r/min. Taking out, drying, placing into a muffle furnace, heating to 1100 deg.C at a rate of 5 deg.C/min, keeping the temperature for 8h, and cooling to room temperature along with the furnace.
2) Washing with deionized water and performing suction filtration, repeating the washing and the suction filtration for 3 times, adding 60g of 10 wt.% PVA solution into a filter cake, uniformly stirring to obtain slurry, and granulating by using spray drying equipment, wherein the inlet temperature is 240 ℃ and the outlet temperature is 120 ℃;
3) and (3) putting the powder obtained after spray granulation into a muffle furnace, heating to 1400 ℃ at a speed of 3 ℃/min, preserving heat for 3h, and cooling along with the furnace to obtain the lanthanum zirconate spherical powder for thermal spraying. The obtained powder is lanthanum zirconate with a single-phase pyrochlore structure, the particle size distribution is 20-80 mu m, and the fluidity is 47.45s/50 g.
Example 3
1) Lanthanum oxide and zirconium oxide were used as starting materials, with lanthanum oxide purity of 99.8 wt.% and zirconium oxide purity of 99.99 wt.%. 34.16g of lanthanum oxide, 25.84g of zirconium oxide, 33.28g of potassium chloride and 26.72g of sodium chloride are weighed by a balance, added into a ball milling tank together with 240g of zirconium oxide balls and 240mL of ethanol, and ball milled for 2 hours at 480 r/min. Taking out, drying, placing into a muffle furnace, heating to 1200 ℃ at a speed of 5 ℃/min, preserving heat for 4h, and cooling to room temperature along with the furnace.
2) Washing with deionized water and performing suction filtration, repeating the washing and the suction filtration for 3 times, adding 25g of 10 wt.% PVA solution into a filter cake, uniformly stirring to obtain slurry, and granulating by using spray drying equipment, wherein the inlet temperature is 240 ℃ and the outlet temperature is 120 ℃;
3) and (3) putting the powder obtained after spray granulation into a muffle furnace, heating to 1400 ℃ at a speed of 3 ℃/min, preserving heat for 3h, and cooling along with the furnace to obtain the lanthanum zirconate spherical powder for thermal spraying. The obtained powder is lanthanum zirconate with a single-phase pyrochlore structure, the particle size distribution is 20-100 mu m, and the fluidity is 41.55s/50 g.
Example 4
1) Lanthanum oxide and zirconium oxide were used as starting materials, with lanthanum oxide purity of 99.8 wt.% and zirconium oxide purity of 99.99 wt.%. 34.16g of lanthanum oxide, 25.84g of zirconium oxide, 33.28g of potassium chloride and 26.72g of sodium chloride are weighed by a balance, added into a ball milling tank together with 240g of zirconium oxide balls and 240mL of ethanol, and ball milled for 2 hours at 480 r/min. Taking out, drying, placing into a muffle furnace, heating to 1000 ℃ at a speed of 5 ℃/min, preserving heat for 10h, and cooling to room temperature along with the furnace.
2) Washing with deionized water and performing suction filtration, repeating the washing and the suction filtration for 3 times, adding 90g of 10 wt.% PVA solution into a filter cake, uniformly stirring to obtain slurry, and granulating by using spray drying equipment, wherein the inlet temperature is 240 ℃ and the outlet temperature is 120 ℃;
3) and (3) putting the powder obtained after spray granulation into a muffle furnace, heating to 1500 ℃ at a speed of 3 ℃/min, preserving heat for 3h, and cooling along with the furnace to obtain the lanthanum zirconate spherical powder for thermal spraying. The obtained powder is lanthanum zirconate with a single-phase pyrochlore structure, the particle size distribution is 20-100 mu m, and the fluidity is 53.35s/50 g.
The molten salt auxiliary method used in the invention mainly utilizes La at high temperature2O3Dissolving in molten salt to facilitate La2O3And ZrO2While the existence of liquid-phase molten salt avoids excessive growth between particles.
The above-described embodiments are intended to be illustrative, rather than restrictive, and all such changes, modifications, substitutions, combinations, and simplifications that may be made without departing from the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A preparation method of lanthanum zirconate spherical powder for thermal spraying is characterized by comprising the following steps:
1) mixing La with the molar ratio of 1:22O3And ZrO2Uniformly mixing the mixture and a molten salt medium through wet ball milling, drying the mixture, heating to 900-1200 ℃, preserving heat for 4-10 hours, and cooling to room temperature; the molten salt medium is sodium chloride and potassium chloride with the mass ratio of 1: 0.8-1: 1.25;
2) washing the reaction product with water to remove residual molten salt medium, adding a binder and deionized water to obtain slurry, and granulating the slurry by using spray drying equipment to obtain spherical powder;
3) and calcining the prepared spherical powder at high temperature to remove the binder and densify the spherical powder to obtain the lanthanum zirconate spherical powder for thermal spraying.
2. The method for preparing lanthanum zirconate spherical powder for thermal spraying according to claim 1, wherein in the step 1), the La is adopted2O3And ZrO2The mass ratio of the total mass to the molten salt medium is 1: 0.5-1: 1.
3. The method for preparing lanthanum zirconate spherical powder for thermal spraying according to claim 1, wherein in the step 1), the wet ball milling fingersAdding the mixture, zirconia balls and absolute ethyl alcohol into a ball milling tank according to the mass ratio of 1:2:1.578, and carrying out ball milling for 2-6 h at the speed of 300-600 r/min; the mixture is La2O3、ZrO2With a molten salt medium.
4. The method for preparing lanthanum zirconate spherical powder for thermal spraying according to claim 1, wherein in the step 1), the temperature is raised to 900 to 1200 ℃ at a rate of 1 to 10 ℃/min.
5. The method for preparing lanthanum zirconate spherical powder for thermal spraying according to claim 1, wherein in the step 1), the La is adopted2O3Has a purity of 99% or more, ZrO2The purity of (A) is more than 99.8%, and the particle size is 40-500 nm.
6. The preparation method of lanthanum zirconate spherical powder for thermal spraying according to claim 1, characterized in that in the step 2), the washing is carried out by adding the reaction product into deionized water in proportion, stirring for 5-15 minutes, and carrying out suction filtration; repeating the steps of adding deionized water into the obtained filter cake according to the proportion, stirring and filtering for 3-6 times; the step of adding deionized water in proportion refers to adding 150-250 g of reaction product into every 500ml of deionized water.
7. The method for preparing lanthanum zirconate spherical powder for thermal spraying according to claim 1, wherein in the step 2), the binder is a PVA solution with a mass concentration of 10%.
8. The method for preparing lanthanum zirconate spherical powder for thermal spraying according to claim 1, wherein in the step 2), the solid content of the slurry is 50-70% by mass.
9. The method for preparing lanthanum zirconate spherical powder for thermal spraying according to claim 1, wherein in the step 3), the high-temperature calcination treatment is heating to 1300-1500 ℃ at a rate of 1-3 ℃/min, keeping the temperature for 2-5 h, and then cooling with a furnace.
10. The method for preparing spherical lanthanum zirconate powder for thermal spraying according to any one of claims 1 to 9, wherein the grain size of the spherical lanthanum zirconate powder for thermal spraying in the step 3) is 100 to 500nm, and the grain size distribution is 20 to 100 μm.
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| CN112125281A (en) * | 2020-10-28 | 2020-12-25 | 中国科学院上海应用物理研究所 | Method for preparing lanthanide oxide material by using coprecipitation combined with molten salt deposition method and application thereof |
| CN112340777A (en) * | 2020-10-30 | 2021-02-09 | 中科立民新材料（扬州）有限公司 | Method for synthesizing pure lanthanum chromate at low temperature, lanthanum chromate synthesized by method and application of lanthanum chromate |
| CN113582691A (en) * | 2021-08-10 | 2021-11-02 | 陕西天璇涂层科技有限公司 | Preparation method of tungsten/tantalate spherical powder |
| CN113603483A (en) * | 2021-08-06 | 2021-11-05 | 陕西天璇涂层科技有限公司 | Rare earth tantalate YxGd(1-x)TaO4Spherical powder and preparation method thereof |
| CN113683418A (en) * | 2021-08-31 | 2021-11-23 | 昆明理工大学 | Tantalate spherical powder CaMoTa for thermal spraying2O9And method for preparing the same |
| CN113716959A (en) * | 2021-08-10 | 2021-11-30 | 陕西天璇涂层科技有限公司 | Spherical powder for thermal barrier coating and preparation method thereof |
| CN113831124A (en) * | 2021-08-06 | 2021-12-24 | 陕西天璇涂层科技有限公司 | Thermal barrier ceramic coating material and preparation method thereof |
| CN115010171A (en) * | 2022-05-19 | 2022-09-06 | 北京科技大学 | Green preparation method of nano lanthanum zirconate powder |
| CN115925419A (en) * | 2022-12-16 | 2023-04-07 | 辽宁省轻工科学研究院有限公司 | Nano-structure rare earth doped lanthanum zirconate thermal barrier coating material and preparation method thereof |
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| CN103305784A (en) * | 2013-06-27 | 2013-09-18 | 中国铝业股份有限公司 | Preparation method of spherical spinel powder for thermal spraying |
| CN110563035A (en) * | 2019-10-14 | 2019-12-13 | 西北工业大学深圳研究院 | Rare earth zirconate nano powder and preparation method and application thereof |
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| CN112125281A (en) * | 2020-10-28 | 2020-12-25 | 中国科学院上海应用物理研究所 | Method for preparing lanthanide oxide material by using coprecipitation combined with molten salt deposition method and application thereof |
| CN112340777A (en) * | 2020-10-30 | 2021-02-09 | 中科立民新材料（扬州）有限公司 | Method for synthesizing pure lanthanum chromate at low temperature, lanthanum chromate synthesized by method and application of lanthanum chromate |
| CN113603483A (en) * | 2021-08-06 | 2021-11-05 | 陕西天璇涂层科技有限公司 | Rare earth tantalate YxGd(1-x)TaO4Spherical powder and preparation method thereof |
| CN113831124A (en) * | 2021-08-06 | 2021-12-24 | 陕西天璇涂层科技有限公司 | Thermal barrier ceramic coating material and preparation method thereof |
| CN113603483B (en) * | 2021-08-06 | 2022-07-01 | 陕西天璇涂层科技有限公司 | Rare earth tantalate YxGd(1-x)TaO4Spherical powder and preparation method thereof |
| CN113582691A (en) * | 2021-08-10 | 2021-11-02 | 陕西天璇涂层科技有限公司 | Preparation method of tungsten/tantalate spherical powder |
| CN113716959A (en) * | 2021-08-10 | 2021-11-30 | 陕西天璇涂层科技有限公司 | Spherical powder for thermal barrier coating and preparation method thereof |
| CN113582691B (en) * | 2021-08-10 | 2023-03-10 | 陕西天璇涂层科技有限公司 | Preparation method of tungsten/tantalate spherical powder |
| CN113683418A (en) * | 2021-08-31 | 2021-11-23 | 昆明理工大学 | Tantalate spherical powder CaMoTa for thermal spraying2O9And method for preparing the same |
| CN115010171A (en) * | 2022-05-19 | 2022-09-06 | 北京科技大学 | Green preparation method of nano lanthanum zirconate powder |
| CN115925419A (en) * | 2022-12-16 | 2023-04-07 | 辽宁省轻工科学研究院有限公司 | Nano-structure rare earth doped lanthanum zirconate thermal barrier coating material and preparation method thereof |
| CN115925419B (en) * | 2022-12-16 | 2024-04-12 | 辽宁省轻工科学研究院有限公司 | Nano-structure rare earth doped lanthanum zirconate thermal barrier coating material and preparation method thereof |
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