Ultrasonic ceramic probe material for high temperature melts and method for producing same

Abstract

The application provides an ultrasonic ceramic probe material for high-temperature melt and a preparation method thereof, and the preparation method comprises the following steps: configuring a precursor solution, wherein the precursor solution comprises polyborazonane and polysilazane; performing electrostatic spray granulation on the precursor solution to obtain precursor particles; calcining the precursor particles to form spherical particles; performing classification sieving on the spherical particles through 500-mesh and 200-mesh sieves in sequence, then ball milling the 200-mesh sieve particles to obtain an A component, and ball milling the 500-mesh sieve particles to obtain a B component; and mixing the A component and the B component uniformly, and then performing hot isostatic pressing to obtain the ultrasonic ceramic probe material for high-temperature melt. The ultrasonic ceramic probe material can realize long-time, continuous and stable ultrasonic wave output in a high-temperature metal melt.

Description

Technical Field

[0001] This invention relates to the field of ultrasonic processing technology for high-temperature melts, specifically to an ultrasonic ceramic probe material for high-temperature melts and its preparation method. Background Technology

[0002] With the rapid development of modern science and technology, industry is increasingly moving towards intelligence and efficiency. As the demand for high-temperature material properties in industrial sectors grows, high-temperature resistant ultrasonic ceramic probes, as an important testing tool, are finding increasingly widespread applications in aerospace, metallurgical engineering, and energy extraction. Ultrasonic waves are elastic mechanical vibration waves with frequencies ranging from 20kHz to 50MHz. They are characterized by short wavelengths, high frequencies, high energy, high energy density, and strong directivity, and can produce mechanical vibration, cavitation, and thermal effects with the medium. In recent years, scholars worldwide have applied ultrasonic enhancement technology to metallurgy, chemical materials, and environmental remediation, hoping to accelerate reaction processes. However, existing ultrasonic probes often experience performance degradation or even damage at high temperatures, limiting their application in such environments.

[0003] Traditional ultrasonic probes are often made of metals or polymers, but these materials are prone to expansion, softening, or chemical reactions at high temperatures, leading to unstable probe performance and failure to meet the demands of high-temperature environments. However, modern industrial applications often involve harsh environments such as high temperatures and high pressures, where particles and bubbles in the high-temperature melt cause severe wear on the probe surface. Traditional high-temperature resistant materials such as zirconium oxide and alumina still suffer from insufficient wear resistance and low ultrasonic wave transmission efficiency at high temperatures. Therefore, developing a novel high-temperature resistant ultrasonic ceramic probe for use with high-temperature melts has become an urgent problem to solve.

[0004] In summary, in order to meet the requirements of ultrasonic detection in high-temperature environments, it is necessary to develop a new method for preparing high-temperature resistant ultrasonic ceramic probes for high-temperature melts, and to propose a corresponding preparation method to overcome the limitations of existing materials in high-temperature environments and promote the application and development of ultrasonic technology in high-temperature environments.

[0005] A search revealed Chinese invention patent application CN113735563A, which discloses a probe material for ultrasonic metallurgy and its preparation method. The preparation method includes: weighing 20-50 parts of dysprosium oxide, 10-50 parts of silicon nitride, 5-20 parts of yttrium oxide, 5-30 parts of boron nitride, 0.5-5 parts of boron carbide, 0.1-3 parts of aluminum nitride, 0.5-2 parts of calcium oxide, and 0.5-1 parts of silicon oxide, mixing them, stirring evenly, and then sieving to obtain sieved mixture I; mixing mixture I... Ball milling was performed to obtain mixture II. Mixture II was then passed through 500-mesh, 300-mesh, and 200-mesh sieves for grading. Two portions of the 500-mesh mixture, two portions of the 300-mesh mixture, and one portion of the 200-mesh mixture were then taken and mixed with polyethylene glycol, ammonium polyacrylate, and water until homogeneous. The mixture was then spray-granulated and passed through a 200-mesh sieve to obtain sieved powder. The powder was then placed in a mold and pressurized under controlled temperature to form a green body, which was then sintered to obtain the ultrasonic metallurgical probe material. However, the thermal shock resistance and high-temperature resistance of this patent still have significant room for improvement. When used in high-temperature melts, it may damage the probe surface, thus affecting its application. Summary of the Invention

[0006] To address the shortcomings of existing technologies, the purpose of this invention is to provide an ultrasonic ceramic probe material for high-temperature melts and its preparation method.

[0007] According to one aspect of the present invention, a method for preparing an ultrasonic ceramic probe material for high-temperature melts is provided, the method comprising:

[0008] A precursor solution is prepared, the precursor solution comprising polyborazine and polysilazine;

[0009] The precursor solution was subjected to electrostatic spray granulation to obtain precursor particles;

[0010] The precursor particles are calcined to form spherical particles;

[0011] The spherical particles were successively passed through 500-mesh and 200-mesh sieves for classification and sieving. Then, the particles were ball-milled through the 200-mesh sieve to obtain component A, and the particles were ball-milled through the 500-mesh sieve to obtain component B.

[0012] After the A component and the B component are mixed evenly, they are subjected to hot isostatic pressing to obtain an ultrasonic ceramic probe material for high-temperature melts.

[0013] Optionally, the precursor solution comprises:

[0014] A mixed solution is provided, the mixed solution comprising 0.1 to 1 part polyethylene glycol, 20 to 50 parts polyborazine, and 20 to 50 parts polysilazine;

[0015] Weigh out 5-15 parts of yttrium oxide, 10-40 parts of dysprosium oxide, 0.5-2 parts of boron carbide, 0.2-2 parts of aluminum nitride, and 0.2-2 parts of calcium oxide, respectively, and add them to a mixing machine for stirring. After mixing evenly, add the mixture to the prepared solution and stir evenly to obtain the precursor solution.

[0016] Optionally, the precursor solution comprises at least one of the following characteristics:

[0017] - The particle size of yttrium oxide is 50–200 μm;

[0018] - Dysprosium oxide has a particle size of 100–200 μm;

[0019] - The particle size of boron carbide is 3-5 μm;

[0020] - The particle size of aluminum nitride is 5-10 μm;

[0021] - The particle size of calcium oxide is 2-5 mm.

[0022] Optionally, the precursor solution is subjected to electrostatic spray granulation, wherein the spinning voltage of electrostatic spray granulation is 20-26 kV, the receiving distance is 18-25 cm, the temperature is 30-40 °C, the humidity is 20%-30%, the outer shell spray liquid propulsion speed is 0.2-0.5 mL / h, and the inner core spray liquid propulsion speed is 0.15-0.3 mL / h.

[0023] Optionally, the calcination of the precursor particles is carried out at a calcination temperature of 800–1100°C, an inlet air temperature of 250–350°C, an air velocity of 30–35 m / s, and a material feeding speed of 50–100 kg / h.

[0024] Optionally, the process of ball milling the 200-mesh sieve particles to obtain component A includes: taking 5 to 10 parts of 200-mesh sieve particles and adding 2 to 5 parts of epoxy resin for ball milling to obtain component A.

[0025] Optionally, the process of ball milling the 500-mesh sieve particles to obtain component B includes: taking 40-50 parts of 500-mesh sieve particles, adding 10-15 parts of polyamide resin and 15-20 parts of polyethylene glycol, and ball milling to obtain component B.

[0026] Optionally, the particles are ball-milled through a 200-mesh sieve to obtain component A, and the particles are ball-milled through a 500-mesh sieve to obtain component B. The ball-to-material ratio is 5:1 to 10:1, the rotation speed is 400 to 500 r / min, and the ball-milling time is 8 to 12 h.

[0027] Optionally, the A component and the B component are mixed evenly and then subjected to hot isostatic pressing, wherein the hot isostatic pressing pressure is 20-40 MPa, the temperature is 1500-1800℃, and the holding time is 1-2 h.

[0028] According to another aspect of the present invention, an ultrasonic ceramic probe material for high-temperature melts is provided, which is prepared by the above-described method for preparing ultrasonic ceramic probe materials for high-temperature melts.

[0029] Compared with the prior art, the present invention has at least one of the following beneficial effects:

[0030] This invention adds polyborane and polysilazane to a precursor solution, which, after calcination, produces high-purity boron nitride and silicon nitride. These materials can encapsulate particles such as yttrium oxide and dysprosium oxide, thereby effectively improving the high-temperature resistance of the probe material. Electrostatic spray granulation improves the uniformity and stability of the material, while graded ball milling followed by hot isostatic pressing further enhances the material's density. Through the synergistic effect of these steps, the ultrasonic ceramic probe material prepared by this invention can deliver long-term, continuous, and stable ultrasonic output in high-temperature molten metal, showing broad application prospects in the field of high-temperature ultrasound. Attached Figure Description

[0031] Other features, objects, and advantages of the present invention will become more apparent from the following detailed description of non-limiting embodiments with reference to the accompanying drawings:

[0032] Figure 1 This is a schematic flowchart of a method for preparing an ultrasonic ceramic probe material for high-temperature melts according to an embodiment of the present invention;

[0033] Figure 2 This is a schematic diagram of the microstructure of the ultrasonic ceramic probe material when components A and B are graded in one embodiment of the present invention. Detailed Implementation

[0034] The present invention will now be described in detail with reference to specific embodiments. These embodiments will help those skilled in the art to further understand the present invention, but do not limit the invention in any way. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention. These all fall within the scope of protection of the present invention.

[0035] To address the problem of poor high-temperature resistance in existing ultrasonic probe materials, referencing Figure 1 An embodiment of the present invention provides a method for preparing an ultrasonic ceramic probe material for high-temperature melts, comprising:

[0036] S1. Prepare a precursor solution, which includes polyborazine and polysilazine;

[0037] S2. Electrostatic spray granulation is performed on the precursor solution to obtain precursor particles;

[0038] S3. Calcined precursor particles form spherical particles;

[0039] S4. The spherical particles are successively passed through 500-mesh and 200-mesh sieves for classification and sieving. Then, the particles sieved through the 200-mesh sieve are ball-milled to obtain component A, and the particles sieved through the 500-mesh sieve are ball-milled to obtain component B. By selecting 500-mesh and 200-mesh grading and ball milling, particles of different sizes can be separated for gradation, thereby improving the density and stability of the material. The gradation of particles of 500-mesh and 200-mesh sizes can provide a more uniform density and strength distribution, making the material more uniform and fine.

[0040] S5. After mixing component A and component B evenly, the mixture is placed into a mold and subjected to hot isostatic pressing to obtain an ultrasonic ceramic probe material for use in high-temperature melts.

[0041] In some embodiments, in step S1, preparing the precursor solution includes:

[0042] S11, providing a mixed solution comprising 0.1 to 1 part polyethylene glycol, 20 to 50 parts polyboronazine, and 20 to 50 parts polysilazine;

[0043] S12: Weigh out 5-15 parts of yttrium oxide, 10-40 parts of dysprosium oxide, 0.5-2 parts of boron carbide, 0.2-2 parts of aluminum nitride, and 0.2-2 parts of calcium oxide, and add them to a mixer. Stir until homogeneous, then add this mixture to the mixed solution and stir until homogeneous to obtain the precursor solution. The above components can meet the performance requirements of ultrasonic ceramic probe materials, such as high-temperature resistance and thermal crack resistance. The components work together to form a good interfacial bond, while also exhibiting good processing performance and process stability. The precursor solution with this formulation allows for good interfacial bonding between the materials, thereby preparing a probe material with excellent performance advantages.

[0044] Smaller particle sizes increase the interfacial area of ​​the material, enhancing the energy transfer and scattering of ultrasound waves, while larger particle sizes increase the mechanical strength and stability of the probe. In some preferred embodiments, the particle size of yttrium oxide is 50–200 μm, dysprosium oxide is 100–200 μm, boron carbide is 3–5 μm, aluminum nitride is 5–10 μm, and calcium oxide is 2–5 mm. These particle sizes improve the uniformity of particle distribution, resulting in a more uniform material, promoting interfacial bonding between materials, and enhancing the probe's high-temperature resistance and thermal crack resistance.

[0045] To achieve electrostatic spray granulation of the precursor solution, in step S2, the precursor solution is placed into the shell layer and core layer propulsion pumps respectively. Appropriate voltage, receiving distance, spray temperature and humidity are selected, and the propulsion speed of the shell layer and core layer propulsion pumps is adjusted respectively to perform electrostatic spray granulation to obtain precursor particles.

[0046] In some preferred embodiments, the spinning voltage for electrostatic spray granulation is 20–26 kV, the receiving distance is 18–25 cm, the temperature is 30–40 °C, the humidity is 20%–30%, the outer shell spray liquid propulsion speed is 0.2–0.5 mL / h, and the inner core spray liquid propulsion speed is 0.15–0.3 mL / h. By reasonably setting the above process parameters, the formation, dispersion, and drying processes of droplets during spray granulation can be controlled, thereby achieving precise control over the size, morphology, and properties of the resulting particles.

[0047] In some embodiments, a cyclone dynamic calcination furnace is used to dynamically calcine the precursor particles to form spherical particles. The calcination temperature is 800–1100℃, the inlet air temperature is 250–350℃, the air velocity is 30–35 m / s, the material feed rate is 50–100 kg / h, and the calcination time is 30–60 s. The settings of the various process parameters for calcination can control the morphology and size of the resulting spherical particles, which is beneficial for subsequent particle classification and gradation.

[0048] In some embodiments, ball milling 200-mesh sieve particles to obtain component A includes: taking 5-10 parts of 200-mesh sieve particles and adding 2-5 parts of epoxy resin for ball milling to obtain component A. The proportions of 200-mesh sieve particles and epoxy resin are mainly determined based on the uniformity of the mixing of the two substances and the viscosity of the mixture.

[0049] In some embodiments, ball milling 500-mesh sieve particles to obtain component B includes: taking 40-50 parts of 500-mesh sieve particles, adding 10-15 parts of polyamide resin and 10-20 parts of polyethylene glycol, and ball milling to obtain component B. The proportions of the 500-mesh sieve, polyamide resin, and polyethylene glycol are mainly considered in terms of particle dispersibility and compatibility with the 200-mesh sieve particles. The 500-mesh sieve particles will adhere to the surface of the 200-mesh particles in subsequent processes, forming a... Figure 2 This structure can improve the density of the material, thereby optimizing its performance.

[0050] In the above-mentioned classifying ball milling process, the ball-to-material ratio was 5:1 to 10:1, the rotation speed was 400 to 500 r / min, and the milling time was 8 to 12 h. The ball milling parameters were the same for 200-mesh and 500-mesh sieves. The various process parameters of the ball milling can be used to control the particle size, morphology, and properties of the resulting particles.

[0051] In this embodiment of the invention, a graded ball milling method is used to grade components A and B, such as... Figure 2 As shown, Figure 2 The arrangement of components A and B in the material can enhance its density, thereby improving its performance.

[0052] In some preferred embodiments, the hot isostatic pressing (HIP) is performed at a pressure of 20–40 MPa, a temperature of 1500–1800 °C, and a holding time of 1–2 h. This ensures uniform deformation and density of the material, guarantees sufficient deformation and compaction, and controls the degree of crystallinity.

[0053] In the above embodiments of the present invention, by adding various materials such as polyboronazine, polysilazine, yttrium oxide, dysprosium oxide, boron carbide, aluminum nitride, and calcium oxide, a composite effect of materials can be achieved. These materials can play different roles in high-temperature environments. For example, after calcination, polyboronazine and polysilazine can generate high-purity boron nitride and silicon nitride, which encapsulate yttrium oxide, dysprosium oxide, and other particles, effectively improving the high-temperature resistance of the probe material. At the same time, it can improve the thermal conductivity of the material, effectively reduce the concentration of thermal stress, prevent crack propagation, and reduce the thermal cracking tendency of the probe material. By limiting the particle size and using electrostatic spray granulation, precise control of the microstructure of the material can be achieved, improving the uniformity and stability of the material. The particle size distribution is achieved through graded ball milling, and the density and stability of the material are further improved through isothermal static pressing, enhancing the overall performance of the material. This allows the prepared ultrasonic ceramic probe material to output ultrasonic waves continuously and stably for a long time in high-temperature molten metal, showing broad application prospects in the field of ultrasonic melts.

[0054] Another embodiment of the present invention provides an ultrasonic ceramic probe material for high-temperature melts, which is prepared using the above-described method for preparing ultrasonic ceramic probe materials for high-temperature melts. The high-temperature resistant ultrasonic ceramic probe formed using this material exhibits good thermal shock resistance and high-temperature resistance, and has broad application prospects in high-temperature melts.

[0055] The present application's solution will be explained below with reference to specific embodiments. Those skilled in the art will understand that the following embodiments are for illustrative purposes only and should not be construed as limiting the scope of the application. Where specific techniques or conditions are not specified in the embodiments, they are performed according to the techniques or conditions described in the literature in the field or according to the product instructions. Reagents or instruments used without specified manufacturers are all conventional products that can be obtained through commercial channels.

[0056] Example 1

[0057] The ultrasonic ceramic probe material for high-temperature melts provided in this embodiment is prepared by the following steps:

[0058] S1. Weigh 10 parts of yttrium oxide with a particle size of 100 μm, 30 parts of dysprosium oxide with a particle size of 100 μm, 1 part of boron carbide with a particle size of 3 μm, 2 parts of aluminum nitride with a particle size of 8 μm, and 1 part of calcium oxide with a particle size of 3 mm. Add them to a mixing machine and stir. After mixing evenly, add 1 part of polyethylene glycol, 30 parts of polyboronazine, and 30 parts of polysilazine to a mixed solution and stir evenly to obtain a precursor solution.

[0059] S2. The precursor solution is placed into the shell and core layer propulsion pumps respectively. A voltage of 25kV, a receiving distance of 25cm, a temperature of 40℃ and a humidity of 30% are selected. The propulsion speed of the shell layer propulsion pump is adjusted to 0.5mL / h and the propulsion speed of the core layer propulsion pump is adjusted to 0.3mL / h. Electrostatic spray granulation is performed to obtain precursor particles.

[0060] S3. The precursor particles are placed in a cyclone dynamic calcining furnace and calcined at 800℃ for 30s. The inlet air temperature is 250℃, the wind speed is 30m / s, and the material feed rate is 50kg / h to obtain spherical particles.

[0061] S4. The spherical particles are passed through 500 mesh and 200 mesh sieves for classification and sieving. Then, 5 parts of the 200 mesh sieve are added to 2 parts of epoxy resin and ball-milled, which is recorded as component A. 45 parts of the 500 mesh sieve are added to 10 parts of polyamide resin and 15 parts of polyethylene glycol and ball-milled, which is recorded as component B. The ball-milling parameters are: ball-to-material ratio of 5:1, rotation speed of 400 r / min, and ball-milling time of 8 h, to obtain the classified and ball-milled particles.

[0062] S5. Mix component A and component B evenly, put them into a mold, and perform hot isostatic pressing at 30MPa and 1500℃ for 1 hour to obtain high-temperature resistant ultrasonic ceramic probe material.

[0063] Example 2

[0064] The ultrasonic ceramic probe material for high-temperature melts provided in this embodiment is prepared by the following steps:

[0065] S1. Weigh 10 parts of yttrium oxide with a particle size of 100 μm, 30 parts of dysprosium oxide with a particle size of 100 μm, 1 part of boron carbide with a particle size of 3 μm, 2 parts of aluminum nitride with a particle size of 8 μm, and 1 part of calcium oxide with a particle size of 3 mm. Add them to a mixing machine and stir. After mixing evenly, add 1 part of polyethylene glycol, 30 parts of polyboronazine, and 30 parts of polysilazine to a mixed solution and stir evenly to obtain a precursor solution.

[0066] S2. The precursor solution is placed into the shell and core layer propulsion pumps respectively. A voltage of 25kV, a receiving distance of 25cm, a temperature of 40℃ and a humidity of 30% are selected. The propulsion speed of the shell layer propulsion pump is adjusted to 0.5mL / h and the propulsion speed of the core layer propulsion pump is adjusted to 0.3mL / h. Electrostatic spray granulation is performed to obtain precursor particles.

[0067] S3. The precursor particles are placed in a cyclone dynamic calcining furnace and calcined at 1100℃ for 30s. The inlet air temperature is 350℃, the wind speed is 35m / s, and the material feed rate is 100kg / h to obtain spherical particles.

[0068] S4. The spherical particles are passed through 500 mesh and 200 mesh sieves for classification and sieving. Then, 10 parts of the 200 mesh sieve are added to 5 parts of epoxy resin and ball-milled, which is recorded as component A. 50 parts of the 500 mesh sieve are added to 15 parts of polyamide resin and 20 parts of polyethylene glycol and ball-milled, which is recorded as component B. The ball-milling parameters are: ball-to-material ratio of 10:1, rotation speed of 500 r / min, and ball-milling time of 12 h, to obtain the classified and ball-milled particles.

[0069] S5. Mix component A and component B evenly, put them into a mold and perform hot isostatic pressing at 40MPa, temperature 1800℃, and holding time 2h to obtain high temperature resistant ultrasonic ceramic probe material.

[0070] Comparative Example

[0071] The ultrasonic ceramic probe material for high-temperature melts provided in the comparative example is prepared by the following steps:

[0072] S1. Weigh 10 parts of yttrium oxide with a particle size of 200 μm, 30 parts of dysprosium oxide with a particle size of 200 μm, 1 part of boron carbide with a particle size of 4 μm, 2 parts of aluminum nitride with a particle size of 10 μm, and 1 part of calcium oxide with a particle size of 5 mm. Add them to a mixing machine and stir. After mixing evenly, add 1 part of polyethylene glycol and 30 parts of polysilazane mixed solution and stir evenly to obtain the precursor solution.

[0073] S2. The precursor solution is placed into the shell and core layer propulsion pumps respectively. A voltage of 25kV, a receiving distance of 25cm, a temperature of 40℃ and a humidity of 30% are selected. The propulsion speed of the shell layer propulsion pump is adjusted to 0.5mL / h and the propulsion speed of the core layer propulsion pump is adjusted to 0.3mL / h. Electrostatic spray granulation is performed to obtain precursor particles.

[0074] S3. The precursor particles are placed in a cyclone dynamic calcining furnace and calcined at 1000℃ for 30s. The inlet air temperature is 300℃, the wind speed is 30m / s, and the material feed rate is 80kg / h to obtain spherical particles.

[0075] S4. The spherical particles are passed through 500 mesh and 200 mesh sieves for classification and sieving. Then, 5 parts of the 200 mesh sieve are added to 2 parts of epoxy resin and ball-milled, which is recorded as component A. 45 parts of the 500 mesh sieve are added to 10 parts of polyamide resin and 15 parts of polyethylene glycol and ball-milled, which is recorded as component B. The ball-milling parameters are: ball-to-material ratio of 10:1, rotation speed of 500 r / min, and ball-milling time of 12 h, to obtain the classified and ball-milled particles.

[0076] S5. Mix component A and component B evenly, put them into a mold, and perform hot isostatic pressing at 40MPa and 1600℃ for 2 hours to obtain high-temperature resistant ultrasonic ceramic probe material.

[0077] The high-temperature resistant ultrasonic ceramic probe materials prepared in Examples 1, 2, and the comparative examples were subjected to performance tests, and the results are shown in Table 1. The criteria for classifying thermal shock resistance were: flexural strength of the sample after thermal shock (above 750 MPa was excellent, 650 MPa to 750 MPa was good, and below 650 MPa was poor); high-temperature resistance was: above 1200℃ was excellent, 1000℃ to 1200℃ was good, and below 1000℃ was poor; and density was: above 95% was excellent, 90% to 95% was good, and below 90% was poor.

[0078] Table 1 Comparison of the material properties of ultrasonic ceramic probes

[0079] Example 1 excellent excellent excellent Example 2 good excellent good Comparative Example good Difference good

[0080] Based on the performance comparison results of Examples 1 and 2, and the comparative examples, it can be seen that when the yttrium oxide particle size is 100 μm, the dysprosium oxide particle size is 100 μm, and the content of polyboronazine and polysilazine is 30 parts, this particle size and material ratio can obtain a more uniform and dense composite material. The choice of materials also affects the performance. The electrostatic spray voltage is 25 kV, the receiving distance is 25 cm, the temperature is 40 °C, the calcination temperature of the cyclone dynamic calcination furnace is 800 °C, and the inlet air temperature is 250 °C. The selection of process parameters—wind speed of 30 m / s and material feed rate of 50 kg / h—affects the morphology, uniformity, and properties of the prepared material. The ball milling ratio of 5:1, rotation speed of 400 r / min, and milling time of 8 h affect the density and uniformity of the material. When hot isostatic pressing (HIP) is performed at a pressure of 30 MPa, a temperature of 1500 °C, and a holding time of 1 h, the high-temperature melt probes prepared exhibit excellent high-temperature resistance, thermal shock resistance, and density. In the comparative example, polyborazane, which did not contain a boron nitride precursor, was not added. Examples 1 and 2 showed superior high-temperature resistance compared to the comparative example. Furthermore, Example 1 also outperformed the comparative example in terms of thermal shock resistance and density.

[0081] Specific embodiments of the present invention have been described above. It should be understood that the present invention is not limited to the specific embodiments described above, and those skilled in the art can make various modifications or variations within the scope of the claims, which do not affect the essence of the present invention. The above preferred features can be used in any combination without conflict.

Claims

1. A method for preparing an ultrasonic ceramic probe material for high-temperature melts, characterized in that, include: A precursor solution is prepared, the precursor solution comprising polyborazine and polysilazine; The precursor solution was subjected to electrostatic spray granulation to obtain precursor particles; The precursor particles are calcined to form spherical particles; The spherical particles were successively passed through 500-mesh and 200-mesh sieves for classification and sieving. Then, the particles were ball-milled through the 200-mesh sieve to obtain component A, and the particles were ball-milled through the 500-mesh sieve to obtain component B. After the A component and the B component are mixed evenly, they are subjected to hot isostatic pressing to obtain an ultrasonic ceramic probe material for high-temperature melts. The precursor solution comprises: A mixed solution is provided, the mixed solution comprising 0.1 to 1 part polyethylene glycol, 20 to 50 parts polyborazine, and 20 to 50 parts polysilazine; Weigh out 5-15 parts of yttrium oxide, 10-40 parts of dysprosium oxide, 0.5-2 parts of boron carbide, 0.2-2 parts of aluminum nitride, and 0.2-2 parts of calcium oxide respectively, add them to a mixing machine and stir. After mixing evenly, add them to the mixed solution and stir evenly to obtain the precursor solution.

2. The method for preparing ultrasonic ceramic probe material for high-temperature melts according to claim 1, characterized in that, The precursor solution comprises at least one of the following characteristics: - Yttrium oxide has a particle size of 50~200 μm; - Dysprosium oxide has a particle size of 100~200um; - The particle size of boron carbide is 3~5 μm; - The particle size of aluminum nitride is 5~10 μm; - The particle size of calcium oxide is 2~5mm.

3. The method for preparing ultrasonic ceramic probe material for high-temperature melts according to claim 1, characterized in that, The precursor solution is subjected to electrostatic spray granulation, wherein the spinning voltage of electrostatic spray granulation is 20-26 kV, the receiving distance is 18-25 cm, the temperature is 30-40℃, the humidity is 20%-30%, the outer shell spray liquid propulsion speed is 0.2-0.5 mL / h, and the inner core spray liquid propulsion speed is 0.15-0.3 mL / h.

4. The method for preparing ultrasonic ceramic probe material for high-temperature melts according to claim 1, characterized in that, The precursor particles are calcined, wherein the calcination temperature is 800~1100℃, the inlet air temperature is 250~350℃, the wind speed is 30~35m / s, and the material feeding speed is 50~100kg / h.

5. The method for preparing ultrasonic ceramic probe material for high-temperature melts according to claim 1, characterized in that, The process of ball milling 200-mesh sieve particles to obtain component A involves taking 5-10 parts of 200-mesh sieve particles and adding 2-5 parts of epoxy resin for ball milling to obtain component A.

6. The method for preparing ultrasonic ceramic probe material for high-temperature melts according to claim 1, characterized in that, The process of ball milling particles through a 500-mesh sieve to obtain component B involves: taking 40-50 parts of particles through a 500-mesh sieve, adding 10-15 parts of polyamide resin and 10-20 parts of polyethylene glycol, and ball milling to obtain component B.

7. The method for preparing ultrasonic ceramic probe material for high-temperature melts according to claim 1, characterized in that, The particles are ball-milled through a 200-mesh sieve to obtain component A, and the particles are ball-milled through a 500-mesh sieve to obtain component B. The ball-to-material ratio is 5:1 to 10:1, the rotation speed is 400 to 500 r / min, and the ball-milling time is 8 to 12 h.

8. The method for preparing ultrasonic ceramic probe material for high-temperature melts according to claim 1, characterized in that, After the A component and the B component are mixed evenly, they are subjected to hot isostatic pressing (HIP). The HIP pressure is 20-40 MPa, the temperature is 1500-1800℃, and the holding time is 1-2 h.

9. An ultrasonic ceramic probe material for high-temperature melts, characterized in that, It is prepared using the method for preparing ultrasonic ceramic probe material for high-temperature melts as described in any one of claims 1-8.

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