Eu, Gd and Dy co-doped YSZ phosphor material, and preparation method and application thereof

Abstract

The application provides a Eu, Gd and Dy co-doped YSZ phosphor material and a preparation method and application thereof, and relates to the technical field of thermal barrier coating materials. The Eu, Gd and Dy co-doped YSZ phosphor material provided by the application is a cubic crystal phase, and comprises 8wt% of Y2O3, 6wt% of Eu2O3, >0 and <=2wt% of Dy2O3, >0 and <=2wt% of Gd2O3 and a balance of ZrO2, wherein the Y2O3, Eu2O3, Dy2O3 and Gd2O3 are solid-solved into the ZrO2 crystal lattice. In the application, the Gd and Dy are selected to co-sensitize the Eu element as a light-emitting center, a plurality of energy transfer paths are formed, the energy transfer efficiency is improved, and the characteristic peak light-emitting intensity of the YSZ:Eu phosphor material is effectively improved. The application improves the high-temperature phosphor performance of the thermal barrier sensing coating, is beneficial to obtaining a higher signal-to-noise ratio, and improves the upper limit of the temperature measurement and the temperature measurement accuracy of the phosphor temperature measurement technology.

Description

Technical Field

[0001] This invention relates to the field of thermal barrier coating materials technology, and in particular to an Eu, Gd and Dy co-doped YSZ phosphorescent material, its preparation method and application. Background Technology

[0002] Thermal barrier coating (TBC) is a key technology for improving the temperature resistance and thermal efficiency of hot-end components inside aero-engines. Because TBC systems are typically multi-layered heterogeneous structures, and aero-engine blades operate in high-temperature, harsh environments for extended periods, TBC-coated blades are prone to damage and failure under complex thermo-mechanical-chemical coupling conditions, posing a serious safety threat to the reliability of aero-engines. Therefore, rapid assessment and accurate diagnosis of the surface temperature distribution and interfacial temperature gradient of the engine blade TBC system are crucial for improving the safety and reliability of aero-engines.

[0003] To obtain accurate information on the temperature distribution of aero-engine turbine blades, researchers both domestically and internationally have employed various advanced temperature measurement technologies. Among these, thermocouple technology is the most mature, but its installation method is destructive, and the installation of leads limits its application to the temperature measurement of rotating components in aero-engines. Temperature-indicating paint and crystal thermometry both detect thermal history temperatures, but due to their cumbersome procedures, high costs, and low accuracy, they are not suitable for detecting the temperature of aero-engine turbine blade surface coatings. Non-contact temperature measurement technologies such as infrared radiation thermometry, fiber optic thermometry, and ultrasonic thermometry also fail to meet temperature measurement requirements due to unresolved issues such as high background noise, emissivity of the measured object, infrared penetration through ceramic layers, and interference from flame radiation. With the increase in thrust-to-weight ratio, the turbine inlet gas temperature has also increased significantly, and the complex service environment of aero-engines limits the application of traditional temperature characterization technologies.

[0004] To effectively monitor the temperature distribution of high-temperature components in real time, temperature characterization technology based on phosphorescence optical properties is a novel non-contact, non-destructive, and transient response detection technology, and a rapidly developing emerging measurement method in recent years. Compared with traditional methods such as thermocouples, optical thermometers, infrared thermometers, and temperature-measuring paints, phosphorescence thermometry has advantages such as high time resolution, low acquisition difficulty, non-contact measurement, and area distribution measurement. It utilizes the thermal quenching effect in the photoluminescence process of phosphorescent materials to establish a quantitative relationship between phosphorescence signal (intensity / lifetime) and temperature, achieving real-time temperature information monitoring.

[0005] Based on the fact that rare-earth phosphorescent materials can coexist stably with thermoelectric thermal barrier (TBC) under certain conditions, combining phosphorescent thermometry with TBC to develop a thermal barrier sensing coating with real-time temperature monitoring is a feasible method for characterizing the temperature of hot-end components in aero-engines. This thermal barrier sensing coating can function as both a phosphorescent thermometric coating and a thermal barrier coating, combining the functions of a thermal insulation and protective coating while enabling online temperature measurement of the thermal barrier coating. YSZ:Eu (Eu-doped YSZ) is currently a widely used phosphorescent material for thermal barrier sensing coatings. However, due to the high-temperature failure phenomenon of phosphorescent materials themselves and the low signal-to-noise ratio under extreme conditions such as high temperature and high corrosion, the upper limit and accuracy of phosphorescent detection technology are insufficient, limiting the development and application of this method. Summary of the Invention

[0006] The purpose of this invention is to provide a Eu, Gd, and Dy co-doped YSZ phosphorescent material, its preparation method, and its applications. The phosphorescent material provided by this invention, when used in thermal barrier sensing coatings, exhibits excellent high-temperature phosphorescence performance, achieving a higher signal-to-noise ratio, which is beneficial for improving the upper limit of temperature measurement and the detection accuracy of phosphorescent thermometry.

[0007] To achieve the above-mentioned objectives, the present invention provides the following technical solution:

[0008] This invention provides a Eu, Gd, and Dy co-doped YSZ phosphorescent material, which is a cubic crystal phase comprising 8 wt% Y2O3, 6 wt% Eu2O3, >0 and ≤2 wt% Dy2O3, >0 and ≤2 wt% Gd2O3, and the balance ZrO2, wherein the Y2O3, Eu2O3, Dy2O3, and Gd2O3 are dissolved in the ZrO2 lattice.

[0009] Preferably, it comprises 8 wt% Y2O3, 6 wt% Eu2O3, 0.5–1.5 wt% Dy2O3, 0.5–1.5 wt% Gd2O3, and the balance ZrO2.

[0010] Preferably, it comprises 8 wt% Y2O3, 6 wt% Eu2O3, 1 wt% Dy2O3, 1 wt% Gd2O3 and the balance ZrO2.

[0011] This invention provides a method for preparing the Eu, Gd, and Dy co-doped YSZ phosphorescent material described above, comprising the following steps:

[0012] According to the mass ratio of each component in the phosphorescent material, Y2O3 powder, Eu2O3 powder, Dy2O3 powder, Gd2O3 powder and ZrO2 powder were wet ball milled to obtain a slurry;

[0013] The slurry is dried to obtain a mixed powder;

[0014] The mixed powder is pressed into a blank to obtain a green body;

[0015] The preform is subjected to solid-state sintering to obtain the Eu, Gd and Dy co-doped YSZ phosphorescent material.

[0016] Preferably, the solid-phase sintering temperature is 1200–1600°C.

[0017] Preferably, the holding time for solid-state sintering is 4 to 10 hours.

[0018] Preferably, the pressing pressure is 10-15 MPa and the holding time is 50-60 s.

[0019] Preferably, the wet ball milling speed is 200-400 r / min and the time is 6-10 h.

[0020] Preferably, the purity of the Y2O3 powder, Eu2O3 powder, Dy2O3 powder, Gd2O3 powder and ZrO2 powder is ≥99.99%.

[0021] This invention provides the application of Eu, Gd, and Dy co-doped YSZ phosphorescent materials described in the above-described scheme or Eu, Gd, and Dy co-doped YSZ phosphorescent materials prepared by the above-described preparation method in thermal barrier coatings.

[0022] This invention provides an Eu, Gd, and Dy co-doped YSZ phosphorescent material (hereinafter referred to as YSZ:Eu,Gd,Dy phosphorescent material), which is a cubic crystal phase comprising 8 wt% Y₂O₃, 6 wt% Eu₂O₃, >0 and ≤2 wt% Dy₂O₃, >0 and ≤2 wt% Gd₂O₃, and the balance ZrO₂. The Y₂O₃, Eu₂O₃, Dy₂O₃, and Gd₂O₃ are dissolved in the ZrO₂ lattice. This invention selects Gd and Dy elements to co-sensitize the Eu element as the luminescence center, forming multiple energy transfer pathways and improving energy transfer efficiency, thereby effectively enhancing the characteristic peak luminescence intensity of the YSZ:Eu phosphorescent material.

[0023] The results of the examples and comparative examples show that the present invention improves the luminescence performance of phosphorescent materials for YSZ:Eu thermal barrier sensing coatings at both room temperature and high temperature. Under ultraviolet light excitation (395 nm), the YSZ:Eu,Gd,Dy phosphorescent materials prepared by the present invention increase the luminescence intensity at wavelengths of 590±10 nm and 605±10 nm by approximately 1.5 times.

[0024] This invention improves the high-temperature phosphorescence performance of thermal barrier sensing coatings, which is beneficial for obtaining a higher signal-to-noise ratio and is of great significance for improving the temperature measurement range and accuracy of phosphorescence thermometry. Attached Figure Description

[0025] Figure 1 XRD patterns of the YSZ:Eu phosphorescent material prepared in Comparative Example 1 and the YSZ:Eu,Gd,Dy phosphorescent material prepared in Example 1;

[0026] Figure 2 Raman spectra of the YSZ:Eu phosphorescent material prepared in Comparative Example 1 and the YSZ:Eu,Gd,Dy phosphorescent material prepared in Example 1;

[0027] Figure 3 XRD patterns of YSZ:Eu,Gd,Dy phosphorescent material and YSZ prepared in Example 1;

[0028] Figure 4 The emission spectra of the YSZ:Eu phosphorescent material prepared in Comparative Example 1 and the YSZ:Eu,Gd,Dy phosphorescent material prepared in Example 1 are shown under room temperature and high temperature conditions.

[0029] Figure 5 XRD patterns of YSZ:Eu,Gd phosphorescent material and YSZ prepared in Comparative Example 2;

[0030] Figure 6 The emission spectra of the YSZ:Eu,Gd phosphorescent material prepared in Comparative Example 2 and the YSZ:Eu,Gd,Dy phosphorescent material prepared in Example 1 at room temperature;

[0031] Figure 7 XRD patterns of YSZ:Eu,Dy phosphorescent material and YSZ prepared in Comparative Example 3;

[0032] Figure 8 The emission spectra of the YSZ:Eu,Dy phosphorescent material prepared in Comparative Example 3 and the YSZ:Eu,Gd,Dy phosphorescent material prepared in Example 1 at room temperature are shown. Detailed Implementation

[0033] This invention provides a Eu, Gd, and Dy co-doped YSZ phosphorescent material, which is a cubic crystal phase comprising 8 wt% Y2O3, 6 wt% Eu2O3, >0 and ≤2 wt% Dy2O3, >0 and ≤2 wt% Gd2O3, and the balance ZrO2, wherein the Y2O3, Eu2O3, Dy2O3, and Gd2O3 are dissolved in the ZrO2 lattice.

[0034] In this invention, the Eu, Gd and Dy co-doped YSZ phosphorescent material preferably contains 0.5 to 1.5 wt% Dy2O3, more preferably 1 wt%.

[0035] In this invention, the Eu, Gd and Dy co-doped YSZ phosphorescent material preferably contains 0.5 to 1.5 wt% Gd2O3, more preferably 1 wt%.

[0036] This invention selects Gd and Dy elements to co-sensitize Eu element as the luminescence center, forming multiple energy transfer paths and improving energy transfer efficiency. This effectively enhances the characteristic peak luminescence intensity of YSZ:Eu phosphorescent material and optimizes the temperature measurement range and accuracy of the thermal barrier sensing coating.

[0037] This invention provides a method for preparing the Eu, Gd, and Dy co-doped YSZ phosphorescent material described above, comprising the following steps:

[0038] According to the mass ratio of each component in the phosphorescent material, Y2O3 powder, Eu2O3 powder, Dy2O3 powder, Gd2O3 powder and ZrO2 powder were wet ball milled to obtain a slurry;

[0039] The slurry is dried to obtain a mixed powder;

[0040] The mixed powder is pressed into a blank to obtain a green body;

[0041] The preform is subjected to solid-state sintering to obtain the Eu, Gd and Dy co-doped YSZ phosphorescent material.

[0042] Unless otherwise specified, all raw materials used in this invention are commercially available products well known in the art.

[0043] According to the mass ratio of each component in the phosphorescent material, the present invention involves wet ball milling of Y2O3 powder, Eu2O3 powder, Dy2O3 powder, Gd2O3 powder and ZrO2 powder to obtain a slurry.

[0044] In this invention, the particle size of the Y2O3 powder, Eu2O3 powder, Dy2O3 powder, Gd2O3 powder, and ZrO2 powder is preferably in the nanometer range; the purity of the Y2O3 powder, Eu2O3 powder, Dy2O3 powder, Gd2O3 powder, and ZrO2 powder is preferably ≥99.99%.

[0045] In this invention, the dispersion medium used in the wet ball milling is preferably water and ethanol. There are no special requirements for the ratio of water to ethanol; any ratio is acceptable. The purpose of adding ethanol is to improve drying efficiency. The amount of water and ethanol used is sufficient to cover the raw material powder and the surface of the grinding balls. The preferred rotation speed of the wet ball milling is 200–400 r / min, more preferably 250–350 r / min, and the preferred milling time is 6–10 h, more preferably 7–9 h. The preferred ball-to-material ratio in the wet ball milling is 4:1; the preferred grinding balls are zirconia grinding balls with a diameter of 5–15 mm, more preferably a mixture of 5 mm, 10 mm, and 15 mm zirconia grinding balls in a quantity ratio of 5:3:2. The wet ball milling is preferably performed in a planetary ball mill.

[0046] After obtaining the slurry, the present invention dries the slurry to obtain a mixed powder.

[0047] In this invention, the drying temperature is preferably 80°C, and the drying time is not particularly important; it is sufficient to dry the mixed powder until it is completely dry. After drying, this invention preferably further includes grinding and sieving the resulting dried powder, preferably through a 200-mesh sieve.

[0048] After obtaining the mixed powder, the present invention presses the mixed powder into a shape to obtain a blank.

[0049] In this invention, the pressing pressure is preferably 10-15 MPa, more preferably 12-13 MPa; the holding time is preferably 50-60 s. This invention does not have special requirements for the dimensions of the blank; dimensions well-known in the art can be used. In an embodiment of this invention, the blank is a cylindrical block with a diameter of 15 mm and a thickness of 1 mm.

[0050] After obtaining the blank, the present invention performs solid-state sintering on the blank to obtain the Eu, Gd and Dy co-doped YSZ phosphorescent material.

[0051] In this invention, the solid-state sintering temperature is preferably 1200–1600°C, more preferably 1400–1500°C, and the holding time is preferably 4–10 h, more preferably 6–8 h; the solid-state sintering is preferably carried out in an air atmosphere. Preferably, the temperature is first increased to 1000°C at a rate of 3–5°C / min, then increased to the solid-state sintering temperature at a rate of 2–3°C / min, and after solid-state sintering is completed, the temperature is then reduced to room temperature at a rate of 50–100°C / h.

[0052] This invention uses solid-state sintering to dissolve Y2O3, Eu2O3, Dy2O3 and Gd2O3 into the ZrO2 lattice to obtain Eu, Gd and Dy co-doped YSZ phosphorescent materials.

[0053] This invention provides the application of the above-mentioned Eu, Gd and Dy co-doped YSZ phosphorescent material in thermal barrier coatings.

[0054] The Eu, Gd, and Dy co-doped YSZ phosphorescent materials, their preparation methods, and applications provided by this invention are described in detail below with reference to specific embodiments. However, these descriptions should not be construed as limiting the scope of protection of this invention.

[0055] Comparative Example 1

[0056] The preparation method of YSZ:Eu phosphorescent material is as follows:

[0057] Weigh 1.6g of Y2O3 nanoparticles with a purity of 99.99%, 1.2g of Eu2O3 nanoparticles with a purity of 99.99%, and 17.2g of ZrO2 nanoparticles with a purity of 99.99%. Add deionized water and ethanol solution to the above powder raw materials, pour them into a polytetrafluoroethylene ball mill jar, and add zirconium oxide grinding balls with a size of 5-15mm (specifically, the ball sizes are 5mm, 10mm, and 15mm mixed in a quantity ratio of 5:3:2). The ball-to-material ratio is 4:1. Place the assembled ball mill jar into a planetary ball mill and ball mill at a speed of 400r / min for 6 hours.

[0058] The ball-milled slurry was poured into a glass dish and dried in an oven at 80°C for 24 hours. The dried powder was then thoroughly ground in an agate mortar and passed through a 200-mesh sieve to obtain a uniform nano-sized mixed powder. The sieved powder was pressed into tablets (15mm in diameter and 1mm in thickness) at 12MPa for 60 seconds using a tablet press. The pressed tablets were then placed in a resistance furnace and held at 1500°C for 4 hours for a solid-phase reaction. The heating rate was 3°C / min below 1000°C and 2°C / min above 1000°C. After holding at this temperature, the temperature was lowered to room temperature at a rate of 100°C / h to obtain YSZ:Eu phosphorescent material.

[0059] Example 1

[0060] An Eu, Gd, and Dy co-doped YSZ phosphorescent material is prepared by the following method:

[0061] Weigh out 1.6g of Y2O3 nanoparticles with a purity of 99.99%, 1.2g of Eu2O3 nanoparticles with a purity of 99.99%, 0.2g of Gd2O3 nanoparticles with a purity of 99.99%, 0.2g of Dy2O3 nanoparticles with a purity of 99.99%, and 16.8g of ZrO2 nanoparticles with a purity of 99.99%. Add deionized water and ethanol solution to the above powder raw materials, pour them into a polytetrafluoroethylene ball mill jar, and add zirconia grinding balls with a size of 5-15mm (specifically, the ball sizes are 5mm, 10mm, and 15mm mixed in a quantity ratio of 5:3:2), with a ball-to-material ratio of 4:1. Place the assembled ball mill jar into a planetary ball mill and ball mill at a speed of 400r / min for 6 hours.

[0062] The ball-milled slurry was poured into a glass dish and dried in an oven at 80°C for 24 hours. The dried powder was then ground thoroughly in an agate mortar and passed through a 200-mesh sieve to obtain a uniform nano-sized mixed powder. The sieved powder was pressed into tablets (15mm in diameter and 1mm in thickness) at 12MPa for 60 seconds using a tablet press. The pressed tablets were then placed in a resistance furnace and held at 1500°C for 4 hours for a solid-state reaction. The heating rate was 3°C / min below 1000°C and 2°C / min above 1000°C. After holding at this temperature, the temperature was lowered to room temperature at a rate of 100°C / h to obtain Eu, Gd, and Dy co-doped YSZ phosphorescent material, denoted as YSZ:Eu,Gd,Dy phosphorescent material.

[0063] Structural and performance testing:

[0064] (1) XRD test

[0065] XRD and Raman spectroscopy tests were performed on the YSZ:Eu phosphorescent material prepared in Comparative Example 1 and the YSZ:Eu,Gd,Dy phosphorescent material prepared in Example 1. The results are shown in the figure. Figures 1-2 .Depend on Figures 1-2 It can be seen that doping with small amounts of sensitizing elements Gd and Dy does not change the structural properties of YSZ:Eu materials, and the prepared YSZ:Eu and YSZ:Eu,Gd,Dy phosphorescent materials are all cubic phase structures.

[0066] The XRD comparison between the YSZ:Eu,Gd,Dy phosphorescent material prepared in Example 1 and YSZ is shown in the figure. Figure 3 ,Depend on Figure 3 It can be seen that the phosphorescent material has the same crystal structure as the yttrium oxide-stabilized zirconia (YSZ) thermal barrier coating material prepared under the same conditions, both being cubic YSZ phases, indicating that Eu, Gd, and Dy are completely dissolved in the YSZ lattice.

[0067] (2) Emission spectrum

[0068] The emission spectra of the YSZ:Eu,Gd,Dy phosphorescent material prepared in Example 1 were measured at room temperature and high temperature, and compared with the spectra of the undoped YSZ:Eu material in Comparative Example 1. The results are as follows: Figure 4 As shown. At room temperature (left) and high temperature (right), doping with the sensitizing element does not change the emission peak position of Eu; both emit narrow-band characteristic spectra at wavelengths of 590±10 nm and 605±10 nm, respectively, indicating that doping with Gd... 3+ and Dy 3+ The doping effectively improved the luminescence intensity of YSZ:Eu, increasing the luminescence intensity at room temperature and 500℃ by nearly 1.5 times.

[0069] Comparative Example 2

[0070] YSZ:Eu,Gd phosphorescent materials were prepared using the same preparation method and conditions.

[0071] Specifically, weigh 1.6g of Y2O3 nanoparticles with a purity of 99.99%, 1.2g of Eu2O3 nanoparticles with a purity of 99.99%, 0.2g of Gd2O3 nanoparticles with a purity of 99.99%, and 17g of ZrO2 nanoparticles with a purity of 99.99%. Add deionized water and ethanol solution to the above powder raw materials, pour them into a polytetrafluoroethylene ball mill jar, and add zirconia grinding balls with a size of 5-15mm (specifically, the ball sizes are 5mm, 10mm, and 15mm mixed in a quantity ratio of 5:3:2), with a ball-to-material ratio of 4:1. Place the assembled ball mill jar into a planetary ball mill and ball mill at a speed of 400r / min for 6 hours.

[0072] The ball-milled slurry was poured into a glass dish and dried in an oven at 80°C for 24 hours. The dried powder was then thoroughly ground in an agate mortar and passed through a 200-mesh sieve to obtain a uniform nano-sized mixed powder. The sieved powder was pressed into tablets (15mm in diameter and 1mm in thickness) at 12MPa for 60 seconds using a tablet press. The pressed tablets were then placed in a resistance furnace and held at 1500°C for 4 hours for a solid-phase reaction. The heating rate was 3°C / min below 1000°C and 2°C / min above 1000°C. After holding at this temperature, the temperature was lowered to room temperature at a rate of 100°C / h to obtain YSZ:Eu,Gd phosphorescent material.

[0073] Structural and performance testing:

[0074] (1) XRD test

[0075] XRD tests were performed on the YSZ:Eu,Gd phosphorescent material prepared in Comparative Example 2, as shown in the results. Figure 5As shown, the phosphorescent material has the same crystal structure as the yttrium-stabilized zirconia (YSZ) thermal barrier coating material prepared under the same conditions, both being cubic phase structures, indicating that Eu and Gd are completely dissolved in the YSZ host matrix lattice.

[0076] (2) Emission spectrum

[0077] The material in Comparative Example 2 was characterized by spectroscopic features, such as... Figure 6 As shown, the luminescence intensity of the YSZ:Eu,Gd phosphorescent material prepared in Comparative Example 2 at room temperature is relatively weaker than that of the YSZ:Eu,Gd,Dy material developed in this invention, only 50% of that of the material in Example 1. Since the phosphorescent material prepared in Comparative Example 2 at room temperature did not increase the light intensity of YSZ:Eu, it indicates that single doping did not play a sensitizing role, and it would not improve under high temperature conditions. Therefore, this invention did not continue to measure the high-temperature spectrum.

[0078] Comparative Example 3

[0079] YSZ:Eu,Dy phosphorescent materials were prepared using the same preparation method and conditions.

[0080] Specifically, weigh 1.6g of Y2O3 nanoparticles with a purity of 99.99%, 1.2g of Eu2O3 nanoparticles with a purity of 99.99%, 0.2g of Dy2O3 nanoparticles with a purity of 99.99%, and 17g of ZrO2 nanoparticles with a purity of 99.99%. Add deionized water and ethanol solution to the above powder raw materials, pour them into a polytetrafluoroethylene ball mill jar, and add zirconia grinding balls with a size of 5-15mm (specifically, the ball sizes are 5mm, 10mm, and 15mm mixed in a quantity ratio of 5:3:2), with a ball-to-material ratio of 4:1. Place the assembled ball mill jar into a planetary ball mill and ball mill at a speed of 400r / min for 6 hours.

[0081] The ball-milled slurry was poured into a glass dish and dried in an oven at 80°C for 24 hours. The dried powder was then thoroughly ground in an agate mortar and passed through a 200-mesh sieve to obtain a uniform nano-sized mixed powder. The sieved powder was pressed into tablets (15mm in diameter and 1mm in thickness) at 12MPa for 60 seconds using a tablet press. The pressed tablets were then placed in a resistance furnace and held at 1500°C for 4 hours for a solid-phase reaction. The heating rate was 3°C / min below 1000°C and 2°C / min above 1000°C. After holding at this temperature, the temperature was lowered to room temperature at a rate of 100°C / h to obtain YSZ:Eu,Dy phosphorescent material.

[0082] Structural and performance testing:

[0083] (1) XRD test

[0084] XRD tests were performed on the YSZ:Eu,Dy phosphorescent material prepared in Comparative Example 3, as shown in the results. Figure 7 As shown, the phosphorescent material has the same crystal structure as the yttrium-stabilized zirconia (YSZ) thermal barrier coating material prepared under the same conditions, both being cubic phase structures, indicating that Eu and Gd are completely dissolved in the YSZ host matrix lattice.

[0085] (2) Emission spectrum

[0086] The YSZ:Eu,Dy phosphorescent material prepared in Comparative Example 3 was characterized by spectroscopic spectra, such as... Figure 8 As shown, the luminescence intensity of the YSZ:Eu,Dy phosphorescent material prepared in Comparative Example 3 at room temperature is relatively weaker than that of the YSZ:Eu,Gd,Dy material developed in this invention, only 37% of that of the material in Example 1. Since the phosphorescent material prepared in Comparative Example 3 at room temperature did not increase the light intensity of YSZ:Eu, it indicates that single doping did not play a sensitizing role, and it would not improve under high temperature conditions. Therefore, this invention did not continue to measure the high-temperature spectrum.

[0087] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A Eu, Gd, and Dy co-doped YSZ phosphorescent material, characterized in that, It is a cubic crystal phase, composed of 8 wt% Y2O3, 6 wt% Eu2O3, >0 and ≤2 wt% Dy2O3, >0 and ≤2 wt% Gd2O3 and the balance ZrO2, wherein the Y2O3, Eu2O3, Dy2O3 and Gd2O3 are dissolved in the ZrO2 lattice.

2. The phosphorescent material according to claim 1, characterized in that, It consists of 8 wt% Y2O3, 6 wt% Eu2O3, 0.5~1.5 wt% Dy2O3, 0.5~1.5 wt% Gd2O3 and the balance ZrO2.

3. The phosphorescent material according to claim 1 or 2, characterized in that, It consists of 8 wt% Y2O3, 6 wt% Eu2O3, 1 wt% Dy2O3, 1 wt% Gd2O3 and the balance ZrO2.

4. The method for preparing the Eu, Gd, and Dy co-doped YSZ phosphorescent material according to any one of claims 1 to 3, characterized in that, Includes the following steps: According to the mass ratio of each component in the phosphorescent material, Y2O3 powder, Eu2O3 powder, Dy2O3 powder, Gd2O3 powder and ZrO2 powder were wet ball milled to obtain a slurry; The slurry is dried to obtain a mixed powder; The mixed powder is pressed into a blank to obtain a green body; The preform is subjected to solid-state sintering to obtain the Eu, Gd and Dy co-doped YSZ phosphorescent material.

5. The preparation method according to claim 4, characterized in that, The solid-state sintering temperature is 1200~1600℃.

6. The preparation method according to claim 4 or 5, characterized in that, The holding time for solid-state sintering is 4 to 10 hours.

7. The preparation method according to claim 4, characterized in that, The pressing pressure is 10~15MPa, and the holding time is 50~60s.

8. The preparation method according to claim 4, characterized in that, The wet ball milling speed is 200~400 r / min, and the time is 6~10 h.

9. The preparation method according to claim 4, characterized in that, The purity of the Y2O3 powder, Eu2O3 powder, Dy2O3 powder, Gd2O3 powder and ZrO2 powder is ≥99.99%.

10. The application of the Eu, Gd and Dy co-doped YSZ phosphorescent material according to any one of claims 1 to 3 or the Eu, Gd and Dy co-doped YSZ phosphorescent material prepared by the preparation method according to any one of claims 4 to 9 in thermal barrier coatings.

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