A high-temperature temperature-pressure field synchronous testing method based on Y2O3:Eu,Er intelligent phosphor layer

Abstract

This invention relates to a method for simultaneous high-temperature and pressure field testing based on a Y₂O₃:Eu,Er smart phosphorescent layer. The invention first prepares Y₂O₃:Eu,Er nanocrystalline phosphorescent microspheres using a spray pyrolysis method combined with phase transformation technology. Then, a Y₂O₃:Eu,Er smart phosphorescent layer is prepared on the surface of the object under test using plasma spraying technology. A laser light source is used to excite the Y₂O₃:Eu,Er smart phosphorescent layer to generate phosphorescence, and dual CCD cameras are used to collect data on the Eu phosphorescence. 3+ and Er 3+ Phosphorescent images were obtained using the two-frame lifetime method. 3+ Phosphorescent lifetime field, via Eu 3+ and Er 3+ Phosphorescent images compared to Eu 3+ / Er 3+ Intensity ratio field. Based on Er 3+ Temperature information was obtained from the phosphorescence lifetime-temperature calibration curve; at the calibration temperature, based on Eu... 3+ / Er 3+ Pressure information is obtained from the intensity ratio-pressure calibration curve, enabling simultaneous measurement of the temperature and pressure fields. Compared with organic temperature- and pressure-sensitive paints, this invention avoids the chemical interactions and energy transfer problems present in existing dual-emissivity mixed phosphorescent layers, as well as the temperature correction error problems present in double-layer phosphorescent layers. It offers high measurement accuracy and is suitable for high-temperature corrosive environments.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of inorganic optical materials, and relates to a high-temperature temperature-pressure field synchronous measurement method based on a Y2O3:Eu,Er intelligent phosphor layer. BACKGROUND

[0002] In the research of aerodynamic problems of hypersonic vehicles and power machines (aircraft engines, gas turbines), surface pressure is one of the most basic and important parameters. Surface pressure measurement can provide key information of many flow field characteristics, significantly improve the understanding and in-depth understanding of researchers on complex flow fields, and provide very valuable data for blade and aircraft shape design and optimization. Pressure-sensitive paint (PSP) based on the photoluminescence process of organic high molecular fluorescent molecules has been used for surface pressure field measurement. Pressure-sensitive paint is composed of organic fluorescent molecules and polymer adhesives. Due to the inherent instability of organic matter, the working temperature of pressure-sensitive paint is generally lower than 200 DEG C.

[0003] High-temperature pressure phosphor coatings based on rare earth ion-doped ceramic materials are considered as important candidate materials for replacing pressure-sensitive paint to achieve surface pressure measurement of higher working temperature components (≥200 DEG C) such as aircraft engines, gas turbines and hypersonic vehicles. However, the high-temperature pressure phosphor coatings found at present have both pressure sensitivity and temperature sensitivity, and the temperature sensitivity is much greater than the pressure sensitivity, which leads to a huge pressure error caused by a small amount of temperature change when high-temperature pressure measurement is performed. The best solution to this defect is to combine high-temperature pressure-sensitive coating and temperature-sensitive coating to form a dual-sensing system, realize temperature and pressure joint measurement, and reduce temperature measurement error.

[0004] In the existing temperature and pressure joint measurement technology, one is to uniformly mix two phosphor materials to form a single-layer double-component phosphor layer, but in this way, the two phosphor materials inevitably have a certain degree of spectral interference, which leads to the decrease of pressure sensitivity of high-temperature pressure-sensitive coating and unnecessary pressure sensitivity of temperature-sensitive coating, and there may be chemical interaction and energy transfer problems between the two phosphor materials, which changes the temperature / pressure sensitivity; the other is to form a double-layer phosphor layer with a pressure-sensitive layer as the surface layer and a temperature-sensitive layer as the inner layer, which is physically isolated, can prevent chemical reaction and energy transfer from mixing, but the surface pressure-sensitive layer will cause the phosphor signal of the temperature-sensitive layer to attenuate, and there is a temperature gradient between the pressure-sensitive layer and the temperature-sensitive layer, which will cause temperature correction error of the pressure-sensitive layer.

[0005] The Chinese invention patent with the authorization number CN107655589A discloses a temperature and pressure combined measurement system and a measurement method. The system comprises a temperature and pressure probe, a fiber coupler connected with the temperature and pressure probe, a laser light source connected with the fiber coupler inlet through the fiber, a beamsplitter connected with the fiber coupler outlet through the fiber, and a signal processing unit arranged behind different light paths of the beamsplitter. The surface of the temperature and pressure probe is coated with Zr3Y4O 12 : Eu mixed phosphor layer. The patent has the advantages of combined measurement of temperature field and pressure field, high temperature measurement (500-1000℃), high accuracy of temperature and pressure measurement, adaptation to temperature and pressure measurement in different environments by changing the shape of the temperature and pressure measurement probe, no influence on the temperature field and the pressure field, wide application range, and application to measurement of temperature and pressure of an aero-engine or a ground gas turbine in a working state. However, the temperature and pressure probe belongs to a contact type measurement technology, and a temperature and pressure probe needs to be pre-prepared in the aero-engine or the ground gas turbine. Moreover, the temperature and pressure of the surrounding environment (i.e. single point) can only be measured. In addition, the phosphorescent signal wavelength range of Zr3Y4O 12 : Eu and MFG phosphor material is very close and overlaps. The phosphorescent peak wavelength range of Zr3Y4O 12 : Eu is 580-640nm, and the phosphorescent peak wavelength range of MFG is 620-670nm. The phosphorescent signal of Zr3Y4O 12 : Eu and the phosphorescent signal of MFG are difficult to separate and interfere with each other, resulting in Zr3Y4O 12 : Eu pressure sensitive characteristics decrease and MFG generates pressure sensitive characteristics that should not exist; Zr3Y4O 12 : Eu and MFG may have chemical interaction and element diffusion at high temperature, resulting in changes in composition. The above defects will seriously affect the accuracy of temperature and pressure measurement.

[0006] Therefore, it is urgent to develop a new type of high-temperature pressure and temperature dual sensing system to solve the existing problems and meet the high-precision synchronous measurement requirements of high-temperature pressure and temperature of hypersonic aircraft and power machinery. The present application proposes a high-temperature pressure and temperature dual sensitive phosphor layer based on Eu 3+ and Er 3 + co-doped yttrium oxide (Y2O3: Eu, Er), which has stable chemical composition and no signal interference, and can obtain excellent pressure and temperature measurement performance. SUMMARY

[0007] The purpose of the present application is to propose a high-temperature temperature and pressure field synchronous test method based on a Y2O3: Eu, Er intelligent phosphor layer.

[0008] The object of the present application can be achieved by the following technical solutions:

[0009] First, Y2O3:Eu, Er nanocrystal phosphor spheres are prepared by a spray pyrolysis method combined with a phase inversion technique, and a Y2O3:Eu, Er intelligent phosphor layer is prepared on the surface of a measured object by a plasma spraying technique; a laser light source is used to excite the Y2O3:Eu, Er intelligent phosphor layer to generate phosphor, and a double-CCD camera is used to collect phosphor images of Eu 3+ and Er 3+ , respectively; an Er 3+ phosphor lifetime field is obtained by a double-frame lifetime method, and an Eu 3+ / Er 3+ intensity ratio field is obtained by comparing Eu 3+ and Er 3+ phosphor images; temperature information is obtained based on an Er 3+ phosphor lifetime-temperature calibration curve; at a calibrated temperature, pressure information is obtained based on an Eu 3+ / Er 3+ intensity ratio-pressure calibration curve, so that temperature-pressure field synchronous measurement is realized; the composition of Y2O3:Eu, Er is (70-90) mol% Y2O3 + (5-20) mol% Eu2O3 + (2-10) mol% Er2O3; the average particle size of the Y2O3:Eu, Er nanocrystal phosphor spheres is 30-120 μm, and the grain size is 30-100 nm; and the thickness of the Y2O3:Eu, Er intelligent phosphor layer is 10-120 μm.

[0010] The specific steps for preparing the Y2O3:Eu, Er nanocrystal phosphor spheres by the spray pyrolysis method combined with the phase inversion technique are as follows:

[0011] (1) First, Y2O3, Eu2O3 and Er2O3 powders in a certain molar ratio are placed in a beaker, a small amount of deionized water and a certain amount of HNO3 are added, and magnetic stirring is performed at 65-75°C for 8-12h, and then a certain amount of deionized water is added and magnetic stirring is performed for 1h, wherein the molar ratio of metal ions to HNO3 is 1:3;

[0012] (2) Then, a certain amount of citric acid is added, and magnetic stirring is performed at 50-70°C for 2-6h for dissolution, and then a certain amount of ethylene glycol is added dropwise under stirring, and magnetic stirring is performed at 100-200°C for 2h to obtain a precursor solution, wherein the molar ratio of metal ions to citric acid is 1:1, and the molar ratio of metal ions to ethylene glycol is 1:(0.5-2);

[0013] (3) then the precursor solution is introduced into the atomizer, the solution is atomized by the atomizer to form an aerosol composed of a large number of small droplets, and is sent into a tube furnace heated to a set temperature (900-1300℃) by air carrier gas (flow rate 6-9 L / min), and after evaporation, drying, decomposition, crystallization reaction and other processes, Eu 3+ co-doped Y2O3:Eu, Er nanocrystalline phosphor powder is obtained. 3+ co-doped Y2O3:Eu, Er nanocrystalline phosphor powder is obtained.

[0014] (4) The cellulose acetate, N-methyl-2-pyrrolidone and Y2O3:Eu, Er nanocrystalline phosphor powder are mixed in a certain proportion to form a uniform slurry, and then the mixed slurry is left to stand for 2-24 h, and a vacuum pump is used to remove the bubbles in the slurry, wherein the mass fraction of cellulose acetate is 5-15%, the mass fraction of N-methyl-2-pyrrolidone is 50-70%, and the mass fraction of Y2O3:Eu, Er nanocrystalline phosphor powder is 25-35%;

[0015] (5) After that, the slurry is poured into the needle cylinder of the electro-spraying peristaltic pump, and the slurry is slowly and uniformly sprayed out of the needle hole of the needle cylinder by the peristaltic pump, and the slurry droplets fall into the water and glycerol mixed solution to form small balls in solid form, wherein the mass ratio of water to glycerol is 1:0.5-2;

[0016] (6) After the solid small balls are dried, they are placed in a high-temperature furnace for calcination at 900-1300℃, and then the calcined solid small balls are sieved to obtain Y2O3:Eu, Er nanocrystalline phosphor small balls.

[0017] The specific steps of preparing the Y2O3:Eu, Er intelligent phosphor layer on the surface of the object to be tested by the plasma spraying technology are as follows:

[0018] (1) The surface to be sprayed is sequentially cleaned with acetone and anhydrous ethanol, and then is placed in an oven at 80-100℃ for drying for 2 h;

[0019] (2) The cleaned surface to be sprayed is subjected to sandblasting treatment on a sandblasting machine using 16-120 mesh corundum sand and a sandblasting pressure of 0.1-0.8 MPa;

[0020] (3) fixing the surface to be sprayed, preheating the surface to be sprayed 2-4 times before spraying, and spraying the Y2O3:Eu, Er intelligent phosphor layer by using the plasma spraying method, wherein the plasma spraying parameters are as follows: the temperature of the substrate is controlled to be 200-650℃, the distance between the spraying gun and the substrate is 80-200mm, the moving speed of the spraying gun is 200-800mm / s, the powder feeding speed is 20-80g / min, the powder feeding gas flow is 0.5-1.5L / min, the spraying voltage is 100-180V, the spraying current is 200-250A, the argon flow rate is 60-150L / min, and the hydrogen flow rate is 20-50L / min.

[0021] the Er 3+ phosphor lifetime field and the temperature information obtained based on the Er 3+ phosphor lifetime-temperature calibration curve are obtained by the double-frame lifetime method.

[0022] (1) a signal generator is used to control the laser light source to emit pulsed laser light with a pulse width of 1-5ms and a pulse period of 10-1000ms, wherein the wavelength of the laser light source is 380-532nm, and the power is 0-10w;

[0023] (2) the Y2O3:Eu, Er intelligent phosphor layer emits phosphor signals under the excitation of the pulsed laser light source;

[0024] (3) a CCD camera is controlled to collect phosphor images at the same time when the laser light source is excited, wherein a band-pass filter with a wavelength of 550±25nm is arranged in front of the CCD camera, and the CCD camera has a double-exposure function and can realize continuous collection of two images in a very short time;

[0025] (4) two phosphor images are continuously collected on the phosphor decay curve generated by the excitation of the pulsed laser light source, wherein the exposure time of the first phosphor image is close to the phosphor lifetime of the material, so that the light intensity of the two phosphor images is close, and the problem of too low signal-to-noise ratio of a certain image is avoided;

[0026] (5) the phosphor lifetime of Er 3+ is determined by the ratio of the light intensity of the corresponding positions in the two phosphor images, and then the temperature information of the position is obtained by the phosphor lifetime-temperature calibration curve of Er 3+ , and a two-dimensional temperature field is obtained; in order to eliminate the interference of background thermal radiation in a high-temperature environment, two background images (I3, I4) are collected with the same exposure time after the collection of the two phosphor images (I1, I2), the corresponding background image (I3, I4) is subtracted from the two phosphor images (I1, I2) respectively, and then the intensity ratio is calculated, and finally the temperature information is obtained.

[0027] the Eu 3+and Er 3+ Phosphor images are obtained 3+ / Er 3+ Intensity ratio field and based on Eu 3+ / Er 3+ The specific steps of obtaining pressure information by the intensity ratio-pressure calibration curve are as follows:

[0028] (1) The Y2O3:Eu,Er smart phosphor layer is excited to emit a phosphor signal using a continuous laser light source, wherein the wavelength of the laser light source is 380-532 nm, and the power is 0-10 w;

[0029] (2) Two CCD cameras are synchronously controlled to collect phosphor images at the same time when the laser light source is excited, one of the CCD cameras is provided with a band-pass filter with a wavelength of 600±25 nm and is used to collect the phosphor image of Eu 3+ , and the other CCD camera is provided with a band-pass filter with a wavelength of 550±25 nm and is used to collect the phosphor image of Er 3+ ;

[0030] (3) The ratio of the intensities of the two phosphor images is calculated and calibrated to obtain the Eu 3+ / Er 3+ intensity ratio at each position;

[0031] (4) According to the Eu 3+ / Er 3+ intensity ratio-pressure calibration curve at the calibrated temperature, the pressure information at the position is obtained, and then a two-dimensional pressure field is obtained.

[0032] Compared with the prior art, the present application has the following advantages:

[0033] 1) The Y2O3:Eu,Er smart phosphor layer used in the present application can realize synchronous measurement of a two-dimensional temperature and pressure field, and the high-temperature-resistant inorganic phosphor coating can realize measurement in a high-temperature environment (800-1400℃);

[0034] 2) Compared with a double-luminescent group mixed phosphor layer composed of different phosphor materials, the Y2O3:Eu,Er phosphor coating has better phase compatibility and chemical stability, and the Y2O3:Eu,Er is prepared by a spray pyrolysis method, so that Eu 3+ and Er 3+ are mixed uniformly at an atomic level;

[0035] 3) The spray pyrolysis method combined with phase inversion electrospinning technology can obtain small balls with excellent fluidity and nanoscale structure, and then the plasma spraying technology is used to obtain a micro-nano double-scale hierarchical structure, and the reflection-enhanced phosphor signal principle is used to significantly improve the temperature and pressure measurement accuracy;

[0036] 4) Compared with existing double-layer phosphorescent layers, since the temperature information and temperature-pressure correlation information are obtained at the same location in the Y2O3:Eu,Er smart phosphorescent layer, the accuracy of temperature correction is ensured.

[0037] 5) Because the Y2O3:Eu,Er smart phosphorescent layer is relatively thin, it has a smaller temperature difference along the thickness direction, which results in higher measurement accuracy;

[0038] 6) Due to Er 3+ The phosphorescence spectrum is 500-575nm, Eu 3+ The phosphorescence spectrum is in the range of 575-650nm. The phosphorescence spectra of the two do not overlap, so there will be no spectral interference, which significantly improves the stability and accuracy of temperature and pressure measurements.

[0039] 7) This phosphorescent coating is suitable for measuring the temperature and pressure fields of rotating parts. It can also be used in very harsh environments such as engine turbines and combustion chambers. It has high measurement accuracy, wide applicability, and good application prospects. Attached Figure Description

[0040] Figure 1 This is a flowchart of a method for synchronous testing of high-temperature and pressure fields based on a Y2O3:Eu,Er smart phosphorescent layer proposed in this invention. Detailed Implementation

[0041] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to specific embodiments.

[0042] Example 1

[0043] First, Y₂O₃:Eu,Er nanocrystalline phosphorescent microspheres were prepared using a spray pyrolysis method combined with phase transformation technology. Then, a Y₂O₃:Eu,Er intelligent phosphorescent layer was prepared on the surface of the object under test using plasma spraying technology. A 395nm laser light source was used to excite the Y₂O₃:Eu,Er intelligent phosphorescent layer to produce phosphorescence. A dual CCD camera was used to collect data on the Eu phosphorescence. 3+ and Er 3+ Phosphorescent images were obtained using the two-frame lifetime method. 3+ Phosphorescent lifetime field, via Eu 3+ and Er 3+ Phosphorescent images compared to Eu 3+ / Er 3+ Intensity ratio field; based on Er 3+ Temperature information was obtained from the phosphorescence lifetime-temperature calibration curve; at the calibration temperature, based on Eu... 3+ / Er 3+ Pressure information is obtained from the intensity ratio-pressure calibration curve, enabling simultaneous measurement of temperature and pressure fields.

[0044] wherein the composition of Y2O3:Eu,Er is 90 mol% Y2O3 + 5 mol% Eu2O3 + 5 mol% Er2O3.

[0045] In this embodiment, the average particle size of the Y2O3:Eu,Er nanocrystal phosphor beads is 40 μm, and the grain size is 30-100 nm; the thickness of the Y2O3:Eu,Er smart phosphor layer is 80 μm.

[0046] In this embodiment, the specific steps for preparing the Y2O3:Eu,Er nanocrystal phosphor beads by the spray pyrolysis method combined with the phase inversion technique are as follows:

[0047] (1) First, a certain molar ratio of Y2O3, Eu2O3 and Er2O3 powders is placed in a beaker, a small amount of deionized water and a certain amount of HNO3 are added, and magnetic stirring is performed at 65°C for 12 h. Then a certain amount of deionized water is added and magnetic stirring is performed for 1 h, wherein the molar ratio of metal ions to HNO3 is 1:3;

[0048] (2) Then a certain amount of citric acid is added and magnetic stirring is performed at 50°C for 6 h for dissolution. After sufficient dissolution, a certain amount of ethylene glycol is added dropwise under stirring, and magnetic stirring is performed at 150°C for 2 h to obtain a precursor solution, wherein the molar ratio of metal ions to citric acid is 1:1, and the molar ratio of metal ions to ethylene glycol is 1:1;

[0049] (3) Then the precursor solution is introduced into an atomizer, and the solution is atomized by the atomizer to form an aerosol composed of a large number of small droplets. The aerosol is sent into a tubular furnace heated to a set temperature (1000°C) by air carrier gas (flow rate 6 L / min). After evaporation, drying, decomposition, and crystallization reactions, Eu 3+ and Er 3+ co-doped Y2O3:Eu,Er nanocrystal phosphor powder is obtained.

[0050] (4) Cellulose acetate, N-methyl-2-pyrrolidone, and Y2O3:Eu,Er nanocrystal phosphor powder are mixed in a certain proportion to form a uniform slurry. Then the mixed slurry is allowed to stand for 12 h, and a vacuum pump is used to remove the air bubbles in the slurry. The mass fraction of cellulose acetate is 10%, the mass fraction of N-methyl-2-pyrrolidone is 60%, and the mass fraction of Y2O3:Eu,Er nanocrystal phosphor powder is 30%.

[0051] (5) Then the slurry is poured into a peristaltic pump syringe for electrospinning, and the slurry is slowly and uniformly sprayed out of the needle hole of the syringe needle by the peristaltic pump. The slurry droplets fall into a mixed solution of water and glycerol, and then precipitate in solid form to form beads, wherein the mass ratio of water to glycerol is 1:1.

[0052] (6) drying the solid small balls and putting them into a high-temperature furnace for sintering at 1100°C, and then sieving the sintered solid small balls to obtain Y2O3:Eu,Er nanocrystal phosphor small balls;

[0053] In this embodiment, the Y2O3:Eu,Er intelligent phosphor layer is prepared on the surface of the object to be measured by plasma spraying technology, and the preparation process is as follows:

[0054] (1) sequentially clean the surface to be sprayed with acetone and anhydrous ethanol, and then dry in an 80°C oven for 2h;

[0055] (2) use 30-mesh corundum sand and a sandblasting pressure of 0.7MPa to perform sandblasting treatment on the cleaned surface to be sprayed on a sandblasting machine;

[0056] (3) fix the surface to be sprayed, preheat the surface to be sprayed three times before spraying, and then spray the Y2O3:Eu,Er intelligent phosphor layer by plasma spraying, wherein the plasma spraying parameters are as follows: the temperature of the substrate is controlled to be 450°C, the distance between the spray gun and the substrate is 100mm, the moving speed of the spray gun is 400mm / s, the powder feeding speed is 40g / min, the powder feeding gas flow is 1L / min, the spraying voltage is 120V, the spraying current is 220A, the argon flow rate is 90L / min, and the hydrogen flow rate is 30L / min.

[0057] In this embodiment, the Er 3+ phosphor lifetime field and the specific steps for obtaining temperature information based on the Er 3+ phosphor lifetime-temperature calibration curve are as follows:

[0058] (1) control the laser light source to emit pulsed laser light with a pulse width of 3ms and a pulse period of 300ms by a signal generator, wherein the wavelength of the laser light source is 395nm and the power is 10w;

[0059] (2) under the excitation of the pulsed laser light source, the Y2O3:Eu,Er intelligent phosphor layer emits phosphor signals;

[0060] (3) control a CCD camera to collect phosphor images at the same time when the laser light source is excited, wherein a band-pass filter with a wavelength of 550±25nm is installed in front of the CCD camera, and the CCD camera has a double-exposure function and can realize continuous collection of two images in a very short time;

[0061] (4) continuously collect two phosphor images on the phosphor decay curve generated by the excitation of the pulsed laser light source, wherein the exposure time of the first phosphor image is close to the phosphor lifetime of the material, so that the light intensity of the two phosphor images is close, and the problem of too low signal-to-noise ratio of a certain image is avoided;

[0062] (5) Determine Er by the ratio of light intensity at corresponding positions in two phosphorescence images. 3+ The phosphorescence lifetime, and then through Er 3+ The temperature information at this location is obtained by the phosphorescence lifetime-temperature calibration curve, and then a two-dimensional temperature field is obtained. In order to eliminate the interference of background thermal radiation under high temperature environment, after the acquisition of two phosphorescence images (I1, I2), two background images (I1, I2) are acquired with the same exposure time. The corresponding background images (I1, I2) need to be subtracted from the two phosphorescence images (I1, I2) respectively, and then the intensity ratio is calculated to finally obtain the temperature information.

[0063] In this embodiment, through Eu 3+ and Er 3+ Phosphorescent images compared to Eu 3+ / Er 3+ Intensity ratio field and Eu-based 3+ / Er 3+ The specific steps for obtaining pressure information from the strength ratio-pressure calibration curve are as follows:

[0064] (1) A continuous laser light source is used to excite the Y2O3:Eu,Er smart phosphorescent layer to emit phosphorescent signals, wherein the wavelength of the laser light source is 395nm and the power is 5W;

[0065] (2) Two CCD cameras are synchronously controlled to acquire phosphorescent images while being excited by a laser light source. One CCD camera is equipped with a 600±25nm bandpass filter for acquiring Eu. 3+ The phosphorescent image was obtained by using a separate CCD camera equipped with a 550±25nm bandpass filter to capture Er. 3+ Phosphorescent images;

[0066] (3) Calculate and calibrate the ratio of the intensities of the two phosphorescent images to obtain the Eu at each location. 3+ / Er 3+ Strength ratio;

[0067] (4) Based on the calibration temperature, Eu 3+ / Er 3+ The intensity ratio-pressure calibration curve is used to obtain the pressure information at that location, and then a two-dimensional pressure field is obtained.

[0068] Example 2

[0069] First, Y₂O₃:Eu,Er nanocrystalline phosphorescent microspheres were prepared using a spray pyrolysis method combined with phase transformation technology. Then, a Y₂O₃:Eu,Er intelligent phosphorescent layer was prepared on the surface of the object under test using plasma spraying technology. A 405nm laser light source was used to excite the Y₂O₃:Eu,Er intelligent phosphorescent layer to produce phosphorescence. A dual CCD camera was used to collect data on the Eu phosphorescence. 3+ and Er3+ Phosphor image of Y2O3:Eu,Er, obtained by double-frame lifetime method 3+ Phosphor lifetime field of Y2O3:Eu,Er, obtained by Eu 3+ and Er 3+ Phosphor image ratio of Y2O3:Eu,Er, obtained by Eu 3+ / Er 3+ Intensity ratio field; based on Er 3+ Phosphor lifetime-temperature calibration curve to obtain temperature information; at the calibration temperature, based on Eu 3+ / Er 3+ Intensity ratio-pressure calibration curve to obtain pressure information, realizing simultaneous measurement of temperature-pressure field.

[0070] wherein the composition of Y2O3:Eu,Er is 80 mol% Y2O 3+ 15 mol% Eu2O 3+ 5 mol% Er2O3.

[0071] In this embodiment, the average particle size of the Y2O3:Eu,Er nanocrystal phosphor beads is 60 μm, and the grain size is 30-100 nm; the thickness of the Y2O3:Eu,Er smart phosphor layer is 120 μm.

[0072] In this embodiment, the specific steps of preparing the Y2O3:Eu,Er nanocrystal phosphor beads by the spray pyrolysis method combined with the phase inversion technique are as follows:

[0073] (1) First, place Y2O3, Eu2O3 and Er2O3 powders in a beaker in a certain molar ratio, add a small amount of deionized water and a certain amount of HNO3, and stir magnetically at 75°C for 8 h, then add a certain amount of deionized water and stir magnetically for 1 h, wherein the molar ratio of metal ions to HNO3 is 1:3;

[0074] (2) Then add a certain amount of citric acid and stir magnetically at 70°C for 2 h to dissolve, and then add a certain amount of ethylene glycol dropwise under stirring conditions, and stir magnetically at 180°C for 2 h to obtain a precursor solution, wherein the molar ratio of metal ions to citric acid is 1:1, and the molar ratio of metal ions to ethylene glycol is 1:2;

[0075] (3) Then introduce the precursor solution into an atomizer, and the solution is atomized by the atomizer to form an aerosol composed of a large number of small droplets, and is sent by air carrier gas (flow rate 9 L / min) into a tubular furnace heated to a set temperature (1000°C), and after evaporation, drying, decomposition, crystallization reaction and other processes, Eu 3+ and Er 3+ co-doped Y2O3:Eu,Er nanocrystal phosphor powder is obtained;

[0076] (4) The cellulose acetate, N-methyl-2-pyrrolidone and Y2O3:Eu, Er nanocrystalline phosphor powder are mixed in a certain proportion to form a uniform slurry, and then the mixed slurry is left to stand for 12 h, and the air bubbles in the slurry are removed using a vacuum pump, wherein the mass fraction of cellulose acetate is 10%, the mass fraction of N-methyl-2-pyrrolidone is 60%, and the mass fraction of Y2O3:Eu, Er nanocrystalline phosphor powder is 30%;

[0077] (5) Then the slurry is poured into a peristaltic pump syringe for electro-spraying, and the slurry is slowly and uniformly sprayed out of the needle hole of the syringe using a peristaltic pump, and the slurry droplets fall into a mixed solution of water and glycerol to form small balls in solid form, wherein the mass ratio of water to glycerol is 1:1;

[0078] (6) The solid small balls are dried and then placed in a high-temperature furnace for calcination at 1100℃, and then the calcined solid small balls are sieved to obtain Y2O3:Eu, Er nanocrystalline phosphor small balls;

[0079] In this embodiment, a Y2O3:Eu, Er intelligent phosphor layer is prepared on the surface of the object to be measured by plasma spraying technology, and the preparation process is as follows:

[0080] (1) The surface to be sprayed is sequentially cleaned with acetone and anhydrous ethanol, and then placed in an 80℃ oven for drying for 2 h;

[0081] (2) The cleaned surface to be sprayed is subjected to sandblasting treatment on a sandblasting machine using 30-mesh corundum sand and a sandblasting pressure of 0.7 MPa;

[0082] (3) The surface to be sprayed is fixed, and the surface to be sprayed is preheated for 3 times before spraying, and then the Y2O3:Eu, Er intelligent phosphor layer is sprayed by plasma spraying method, wherein the plasma spraying parameters are as follows: the temperature of the substrate is controlled at 500℃, the distance between the spray gun and the substrate is 120 mm, the moving speed of the spray gun is 500 mm / s, the powder feeding speed is 50 g / min, the powder feeding gas flow is 1.5 L / min, the spraying voltage is 150 V, the spraying current is 250 A, the argon flow rate is 120 L / min, and the hydrogen flow rate is 50 L / min.

[0083] In this embodiment, Er 3+ phosphor lifetime field and the specific steps for obtaining temperature information based on the Er 3+ phosphor lifetime-temperature calibration curve are as follows:

[0084] (1) A pulse laser with a pulse width of 3 ms and a pulse period of 300 ms is emitted by a signal generator, wherein the wavelength of the laser light source is 405 nm and the power is 10 w;

[0085] (2) Y2O3:Eu,Er smart phosphor layer emits phosphor signal under the excitation of pulsed laser light source;

[0086] (3) Control a CCD camera to collect phosphor images at the same time when the laser light source is excited. The CCD camera is equipped with a band-pass filter of 550±25nm. The CCD camera has a double exposure function, which can realize the continuous collection of two images in a very short time.

[0087] (4) Collect two phosphor images on the phosphor decay curve generated by the excitation of pulsed laser light source. The exposure time of the first phosphor image is close to the phosphor lifetime of the material, so that the light intensity of the two phosphor images is close, avoiding the problem that the signal-to-noise ratio of a certain image is too low.

[0088] (5) Determine the phosphor lifetime of Er 3+ by the ratio of light intensity at corresponding positions in two phosphor images, and then obtain the temperature information of the position through the phosphor lifetime-temperature calibration curve of Er 3+ , and further obtain the two-dimensional temperature field. In order to eliminate the interference of background thermal radiation in high temperature environment, two background images (I1, I2) are collected with the same exposure time after the collection of two phosphor images (I1, I2). The intensity ratio is calculated after the two phosphor images (I1, I2) are respectively subtracted from the corresponding background images (I1, I2). Finally, the temperature information is obtained.

[0089] In this embodiment, the specific steps of obtaining the Eu 3+ / Er 3+ intensity ratio field and the pressure information based on the Eu 3+ / Er 3+ intensity ratio-pressure calibration curve through the Eu 3+ / Er 3+ phosphor image ratio are as follows:

[0090] (1) Use a continuous laser light source to excite Y2O3:Eu,Er smart phosphor layer to emit phosphor signal, wherein the wavelength of the laser light source is 405nm and the power is 5w;

[0091] (2) Synchronously control two CCD cameras to collect phosphor images at the same time when the laser light source is excited. One CCD camera is equipped with a band-pass filter of 600±25nm for collecting Eu 3+ phosphor image, and the other CCD camera is equipped with a band-pass filter of 550±25nm for collecting Er 3+ phosphor image;

[0092] (3) Calculate and calibrate the ratio of the intensity of two phosphor images to obtain the Eu 3+ / Er 3+intensity ratio;

[0093] (4) according to the calibration temperature, Eu 3+ / Er 3+ The intensity ratio-pressure calibration curve is obtained, the pressure information of the position is obtained, and then the two-dimensional pressure field is obtained.

[0094] The above is only a specific embodiment of the present application, but the design concept of the present application is not limited thereto, and any non-essential modification of the present application using this concept shall belong to the act of infringing the protection scope of the present application. Any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present application without departing from the technical solutions of the present application still belongs to the protection scope of the technical solutions of the present application.

Claims

1. A method for synchronously testing high-temperature and pressure fields based on a Y₂O₃:Eu,Er smart phosphorescent layer, characterized in that, First, Y₂O₃:Eu,Er nanocrystalline phosphorescent microspheres were prepared using a spray pyrolysis method combined with phase transformation technology. Then, a Y₂O₃:Eu,Er intelligent phosphorescent layer was prepared on the surface of the object under test using plasma spraying technology. A laser light source was used to excite the Y₂O₃:Eu,Er intelligent phosphorescent layer to produce phosphorescence, and dual CCD cameras were used to collect data on the Eu phosphorescence. 3+ and Er 3+ Phosphorescent images were obtained using the two-frame lifetime method. 3+ Phosphorescent lifetime field, via Eu 3+ and Er 3+ Phosphorescent images compared to Eu 3+ / Er 3+ Intensity ratio field; based on Er 3+ Temperature information was obtained from the phosphorescence lifetime-temperature calibration curve; at the calibration temperature, based on Eu... 3+ / Er 3+ Pressure information is obtained through an intensity-pressure calibration curve, enabling synchronous measurement of the temperature-pressure field. The Y2O3:Eu,Er intelligent phosphorescent layer can achieve measurement in high-temperature environments of 800–1400℃. The composition of the Y2O3:Eu,Er is 70-90 mol% Y2O3 + 5-20 mol% Eu2O3 + 2-10 mol% Er2O3. The average particle size of the Y2O3:Eu,Er nanocrystalline phosphorescent microspheres is 30-120 μm, and the crystal size is 30-100 nm. The thickness of the Y2O3:Eu,Er intelligent phosphorescent layer is 10-120 μm.

2. The method according to claim 1, characterized in that, The specific steps for preparing Y2O3:Eu,Er nanocrystalline phosphorescent microspheres using the spray pyrolysis method combined with phase inversion technology are as follows: (1) First, place Y2O3, Eu2O3 and Er2O3 powders in a beaker with a certain molar ratio, add a small amount of deionized water and a quantitative amount of HNO3, and stir magnetically at 65-75℃ for 8-12 hours. Then add a certain amount of deionized water and stir magnetically for 1 hour. The molar ratio of metal ions to HNO3 is 1:

3. (2) Then add a certain amount of citric acid and stir magnetically at 50-70℃ for 2-6 hours to dissolve. After it is fully dissolved, add a certain amount of ethylene glycol dropwise under stirring and stir magnetically at 100-200℃ for 2 hours to obtain a precursor solution. The molar ratio of metal ions to citric acid is 1:1 and the molar ratio of metal ions to ethylene glycol is 1:0.5 to 1:

2. (3) The precursor solution is then introduced into an atomizer. After being atomized, the solution forms an aerosol composed of a large number of tiny droplets. This aerosol is then fed into a tube furnace heated to a set temperature of 900-1300℃ by an air carrier gas at a flow rate of 6-9 L / min. After evaporation, drying, decomposition, and crystallization, Eu is obtained. 3+ With Er 3+ Co-doped Y₂O₃:Eu,Er nanocrystalline phosphorescent powder; (4) Mix cellulose acetate, N-methyl-2-pyrrolidone and Y2O3:Eu,Er nanocrystalline phosphorescent powder in a certain proportion to form a uniform slurry. Then let the mixed slurry stand for 2-24 hours and use a vacuum pump to remove air bubbles from the slurry. The mass fraction of cellulose acetate is 5-15%, the mass fraction of N-methyl-2-pyrrolidone is 50-70%, and the mass fraction of Y2O3:Eu,Er nanocrystalline phosphorescent powder is 25-35%. (5) Then pour the slurry into the peristaltic pump syringe for electric spraying, and use the peristaltic pump to slowly and evenly spray the slurry from the needle hole of the syringe. After the slurry drops into the water and glycerin mixture, it will precipitate in solid form to form small balls. (6) After drying the solid microspheres, they are placed in a high-temperature furnace and calcined at 900-1300℃. Then, the calcined solid microspheres are sieved to obtain Y2O3:Eu,Er nanocrystalline phosphorescent microspheres.

3. The method according to claim 1, characterized in that, The specific steps for preparing the Y2O3:Eu,Er smart phosphorescent layer on the surface of the object to be tested using plasma spraying technology are as follows: (1) Clean the surface to be sprayed with acetone and anhydrous ethanol in sequence, and then dry it in an oven at 80-100℃ for 2 hours; (2) Use 16-120 mesh corundum sand and a sandblasting pressure of 0.1-0.8 MPa to sandblast the cleaned surface to be sandblasted on a sandblasting machine. (3) Fix the surface to be sprayed. Before spraying, preheat the surface to be sprayed 2-4 times. After preheating, use plasma spraying to spray the Y2O3:Eu,Er smart phosphorescent layer. The plasma spraying parameters are as follows: control the temperature of the substrate to be 200-650℃, the distance between the spray gun and the substrate to be 80-200mm, the moving speed of the spray gun to be 200-800mm / s, the powder feeding speed to be 20-80g / min, the powder feeding airflow to be 0.5-1.5L / min, the spraying voltage to be 100-180V, the spraying current to be 200-250A, the argon flow rate to be 60-150L / min, and the hydrogen flow rate to be 20-50L / min.

4. The method according to claim 1, characterized in that, The specific steps for obtaining the Er3+ phosphorescence lifetime field using the dual-frame lifetime method and obtaining temperature information based on the Er3+ phosphorescence lifetime-temperature calibration curve are as follows: (1) The laser source is controlled by a signal generator to emit a pulsed laser with a pulse width of 1-5ms and a pulse period of 10-1000ms, wherein the wavelength of the laser source is 380-532nm and the power is 0-10w; (2) Under the excitation of a pulsed laser source, the Y2O3:Eu,Er smart phosphorescent layer emits phosphorescent signals; (3) Control a CCD camera to acquire phosphorescent images while being excited by a laser light source. The CCD camera is equipped with a 550±25nm bandpass filter. The CCD camera has a double exposure function, which can realize the continuous acquisition of two images in a very short time. (4) Two phosphorescent images are continuously acquired on the phosphorescence decay curve generated by the pulsed laser source. The exposure time of the first phosphorescent image is close to the phosphorescence lifetime of the material, so that the light intensity of the two phosphorescent images is close, avoiding the problem that the signal-to-noise ratio of one image is too low. (5) The phosphorescence lifetime of Er 3+ is determined by the ratio of the light intensity at corresponding positions in two phosphorescence images. Then, the temperature information at that position is obtained by the phosphorescence lifetime-temperature calibration curve of Er 3+, and thus a two-dimensional temperature field is obtained. In order to eliminate the background thermal radiation interference under high temperature environment, after the two phosphorescence images are acquired, two background images are acquired with the same exposure time. The intensity ratio is calculated after subtracting the corresponding background image from the two phosphorescence images, and finally the temperature information is obtained.

5. The method according to claim 1, characterized in that, The aforementioned via Eu 3+ and Er 3+ Phosphorescent images compared to Eu 3 + / Er 3+ Intensity ratio field and Eu-based 3+ / Er 3+ The specific steps for obtaining pressure information from the strength ratio-pressure calibration curve are as follows: (1) A continuous laser light source is used to excite the Y2O3:Eu,Er smart phosphorescent layer to emit phosphorescent signals, wherein the wavelength of the laser light source is 380-532nm and the power is 0-10w; (2) Two CCD cameras are synchronously controlled to acquire phosphorescent images while being excited by a laser light source. One CCD camera is equipped with a 600±25nm bandpass filter for acquiring Eu. 3+ The phosphorescent image was obtained by using a separate CCD camera equipped with a 550±25nm bandpass filter to capture Er. 3+ Phosphorescent images; (3) Calculate and calibrate the ratio of the intensities of the two phosphorescent images to obtain the Eu at each location. 3+ / Er 3+ Strength ratio; (4) Based on the calibration temperature, Eu 3+ / Er 3+ The intensity ratio-pressure calibration curve is used to obtain the pressure information at that location, and then a two-dimensional pressure field is obtained.

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