A Yttrium Fluoride Oxide Spraying Powder, Its Preparation Method and Application

Abstract

This invention belongs to the field of rare earth materials technology, specifically relating to a yttrium oxyfluoride spraying powder, its preparation method, and its application. The preparation method includes the following steps: S1, mixing a soluble yttrium salt, a dispersant, a first solvent, and a precipitant to undergo a precipitation reaction, obtaining a slurry; the precipitant includes carbonates and / or bicarbonates; S2, mixing the slurry and a fluorinating agent to undergo a fluorination reaction, obtaining a yttrium oxyfluoride precursor; S3, mixing the yttrium oxyfluoride precursor, a second solvent, and a binder, ball milling, granulating, and calcining to obtain the yttrium oxyfluoride spraying powder. This invention uses safe and environmentally friendly raw materials with low cost, and the process is simple and efficient, enabling stable industrial production. The obtained yttrium oxyfluoride spraying powder has high purity, regular morphology, concentrated particle size distribution, and good sphericity. When applied in the semiconductor field, it can significantly improve the density, bonding strength, and plasma etching resistance of plasma-sprayed coatings.

Description

Technical Field

[0001] This invention belongs to the field of rare earth materials technology, specifically relating to a yttrium fluoride spraying powder, its preparation method, and its application. Background Technology

[0002] Powders for spraying are widely used in semiconductor equipment manufacturing, flat panel display production equipment, chemical and new energy corrosion-resistant equipment, and aerospace and defense industries. Yttrium oxide-based spherical powders are among the most competitive materials. Yttrium oxide-based powders include yttrium oxide (Y₂O₃), yttrium aluminum silicate (YAS), yttrium aluminum garnet (YAG), yttrium aluminum monoclinic crystal (YAM), yttrium fluoride (YF₃), and yttrium fluoride oxyfluoride (YOF, Y₅O₄F₇, Y₆O₅O₈, Y₇O₆F₉). However, yttrium oxide and aluminum oxide alone are prone to react with fluorine-based gases (HF, CF₄, CHF₃, SF₆, etc.), leading to changes in gas concentration and thus the problem of "process drift." Therefore, yttrium fluoride and yttrium fluoride oxyfluoride powders are preferred. However, during plasma spraying, yttrium fluoride alone is prone to decomposition at 3000℃, and subsequent sprayed coatings are also prone to cracking and particle detachment. Therefore, yttrium oxyfluoride is the preferred powder for spraying. Yttrium oxyfluoride is a stable compound between fluorides and oxides.

[0003] Previously, yttrium oxyfluoride was mostly prepared using solid-phase methods, which involved mixing and grinding yttrium oxide and yttrium fluoride or ammonium fluoride, followed by calcination to obtain yttrium oxyfluoride powder. However, solid-phase methods suffer from drawbacks such as uneven mixing of raw materials, difficulty in controlling product particle size and morphology, high reaction temperatures, and high energy consumption. Therefore, many researchers have begun to focus on liquid-phase (wet chemical) methods to assist in the preparation of yttrium oxyfluoride. However, existing liquid-phase methods for preparing yttrium oxyfluoride use oxalic acid, urea, and hydrofluoric acid, which are hazardous and expensive raw materials. Furthermore, uneven mixing of raw materials leads to irregular morphology or severe agglomeration of the obtained yttrium oxyfluoride, and the plasma corrosion resistance, thermal stability, and electrical insulation properties of the yttrium oxyfluoride fail to meet requirements. Summary of the Invention

[0004] Therefore, in order to solve the above-mentioned technical problems, the present invention provides a yttrium fluoride spraying powder, its preparation method and application.

[0005] In a first aspect, the present invention protects a method for preparing yttrium fluoride spray powder, wherein the preparation method includes the following steps: S1, a soluble yttrium salt, dispersant, first solvent, and precipitant are mixed and subjected to a precipitation reaction to obtain a slurry; The precipitant includes carbonates and / or bicarbonates; S2, the slurry and fluorinating agent are mixed and fluorinated to obtain the yttrium oxyfluoride precursor; S3, the yttrium oxyfluoride precursor, the second solvent, and the binder are mixed, ball-milled, granulated, and calcined to obtain yttrium oxyfluoride spray powder.

[0006] In one optional embodiment, the soluble yttrium salt includes an inorganic soluble yttrium salt; optionally, it includes at least one of yttrium chloride, yttrium acetate, and yttrium nitrate.

[0007] In one optional embodiment, the dispersant comprises an organic dispersant, optionally including at least one of polyethylene glycol, stearic acid, and oleic acid; optionally including at least one of polyethylene glycol 2000, polyethylene glycol 4000, polyethylene glycol 6000, and polyethylene glycol 20000.

[0008] In one optional embodiment, the ratio of the mass of the dispersant to the mass of yttrium in the soluble yttrium salt converted to yttrium oxide is (0.1-3):100. It should be noted that converting the mass of yttrium in the soluble yttrium salt to yttrium oxide is for ease of engineering calculation and does not imply that the soluble yttrium salt itself contains yttrium oxide. For example, when the soluble yttrium salt is yttrium nitrate, a mass converted to yttrium oxide of 10 kg means that the mass of yttrium in yttrium nitrate converted to yttrium oxide is 10 kg. The relative molecular mass of yttrium oxide (Y₂O₃) is 225.81, and the relative atomic mass of yttrium (Y) is 88.91. The mass fraction of Y in Y₂O₃ is approximately (2 × 88.91) / 225.81 ≈ 0.7876. The mass of yttrium in yttrium nitrate is calculated as: (converted mass of yttrium oxide) × 0.7876 = 10 kg × 0.7876 = 7.876 kg. The chemical formula of yttrium nitrate hexahydrate is Y(NO₃)₃·6H₂O, with a relative molecular mass of 380.95. The mass fraction of Y in ·6H2O = 88.91 / 380.95≈0.2334; the actual mass of added yttrium nitrate hexahydrate = mass of yttrium element / 0.2334 = 7.876 kg / 0.2334≈33.75 kg; that is, when the soluble yttrium salt is yttrium nitrate converted to yttrium oxide and the mass is 10 kg, the actual mass of added hexahydrate Y(NO3)3·6H2O is 33.75 kg; for other types of soluble yttrium salts, the conversion is also done in the same way.

[0009] In this invention, the first solvent is a conventional solvent in the art. Typically, but not specifically, the first solvent is water, and conventional laboratory water is sufficient.

[0010] In step S1 of this invention, in order to achieve a more uniform mixing, yttrium nitrate, dispersant, and first solvent can be mixed to obtain a solution, and then a precipitant can be added to carry out a precipitation reaction to obtain a slurry; optionally, the concentration of yttrium ions in the solution is 0.3-0.5 mol / L.

[0011] In step S1 of this invention, in order to make the precipitation reaction more complete, the precipitant and water can be mixed first to prepare a precipitant solution with a concentration of 0.5-4 mol / L before proceeding with subsequent operations.

[0012] In one optional embodiment, the molar ratio of carbonate ions and / or bicarbonate ions to yttrium ions in the soluble yttrium salt is (1-6):1. As an example, the molar ratio of carbonate ions and / or bicarbonate ions to yttrium ions in the soluble yttrium salt can be 1:1, 2:1, 3:1, 4:1, 5:1, 6:1, or within any range of the above values; (2-4):1 is an option.

[0013] In one optional embodiment, the precipitant includes at least one of sodium carbonate, potassium carbonate, ammonium carbonate, sodium bicarbonate, potassium bicarbonate, and ammonium bicarbonate; optionally, it includes ammonium carbonate and / or ammonium bicarbonate.

[0014] In one optional embodiment, the precipitation reaction is carried out at a temperature of 25-60°C for a time of 0.5-3 hours. As an example, the precipitation reaction temperature can be 25°C, 30°C, 40°C, 50°C, 60°C, or any range thereof; the precipitation reaction time can be 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, or any range thereof.

[0015] In step S1 of this invention, after the precipitation reaction, the filter cake is further aged, filtered, washed, and then re-dispersed in the first solvent. This effectively removes reaction byproducts and unreacted precipitants, improves the purity of the precursor filter cake, and provides a uniformly dispersed slurry for the subsequent fluorination reaction. The specific steps are all conventional steps in the art. Typically, without limitation, the aging temperature is room temperature, the time is 10-30 min, and the mass ratio of the filter cake to the first solvent is 1:(1-3).

[0016] In this invention, in order to make the fluorination reaction more complete, the fluorinating agent is mixed with water to prepare a fluorinating agent solution with a concentration of 1-5 mol / L.

[0017] In one optional embodiment, the molar ratio of fluoride ions in the fluorinating agent to yttrium ions in the slurry is (1-2.5):1. As an example, the molar ratio of fluoride ions in the fluorinating agent to yttrium ions in the slurry can be 1:1, 1.5:1, 2:1, 2.5:1, or within any of the above values; it can be (1-1.2):1.

[0018] In one optional embodiment, the fluorinating agent comprises fluorinated organic carboxylic acids and / or fluorinated salts; optionally, it comprises at least one of trifluoroacetic acid, ammonium fluoride, sodium fluoride, and potassium fluoride, and more preferably, ammonium fluoride.

[0019] In this invention, the fluorinating agent has high purity, weak corrosivity, and good safety. It does not contain highly corrosive hydrofluoric acid and does not introduce heavy metals or other harmful impurities during the reaction process. This can further improve the purity of the yttrium oxyfluoride precursor, which is beneficial to improving the purity and particle size of the final yttrium oxyfluoride spray powder, while making the production process more environmentally friendly and safe.

[0020] In one optional embodiment, the fluorination reaction is carried out at a temperature of 25-60°C for a time of 0.5-2 hours. As an example, the temperature of the fluorination reaction can be 25°C, 30°C, 40°C, 50°C, 60°C, or any of the above values; the time of the fluorination reaction can be 0.5 hours, 1 hour, 1.5 hours, 2 hours, or any of the above values.

[0021] In step S2 of this invention, after the fluorination reaction, the steps of filtration, aging, washing, and drying are further performed; this can further remove the byproducts and excess fluorinating agent produced by the fluorination reaction, and obtain a pure yttrium fluoride precursor. The specific steps are all conventional steps in the art. Typically, without limitation, the aging temperature is room temperature, and the aging time is 0.5-3 hours.

[0022] In one optional embodiment, the mass ratio of the yttrium oxyfluoride precursor to the second solvent is (1-6):(4-7).

[0023] In this invention, the second solvent is a conventional solvent in the art. Typically, but not specifically, the second solvent is water, and conventional laboratory water is sufficient.

[0024] In one alternative embodiment, the amount of the binder is 0.1-3 wt% based on the mass of the yttrium oxyfluoride precursor.

[0025] In one alternative embodiment, the adhesive is conventional in the art and includes at least one of cellulose, polyvinyl alcohol, and polyvinylpyrrolidone. Optionally, the cellulose includes at least one of methylcellulose and carboxymethylcellulose.

[0026] In one optional embodiment, the ball mill rotates at 300-600 rpm and grinds until the slurry D50 is below 1 μm.

[0027] In one optional embodiment, the granulation speed is 13000-26000 rpm, the inlet temperature is 200-300℃, the outlet temperature is 100-200℃, and the material pumping speed is 25-50 rpm.

[0028] In one optional embodiment, the granulated particles have a D50 of 15-70 μm and a (D90-D10) / 2×D50 of 0.2-0.7. And / or, the calcination heating rate is 1-5℃ / min, the temperature is 500-1200℃, and the time is 3-10h; as an example, the calcination temperature can be 500℃, 600℃, 800℃, 1000℃, 1200℃, or within any range of the above values; the calcination time can be 3h, 4h, 5h, 6h, 10h, or within any range of the above values; optionally, the temperature is 800-1000℃.

[0029] A second aspect of this invention protects a yttrium fluoride spraying powder prepared by the aforementioned preparation method.

[0030] The third aspect of this invention protects the application of the aforementioned yttrium fluoride spray powder in the semiconductor field.

[0031] The technical solution of this invention has the following advantages: This invention provides a method for preparing yttrium oxyfluoride spraying powder, wherein the preparation method includes the following steps: S1, mixing soluble yttrium salt, dispersant, first solvent, and precipitant to carry out a precipitation reaction to obtain a slurry; the precipitant includes carbonate and / or bicarbonate; S2, mixing the slurry and fluorinating agent to carry out a fluorination reaction to obtain a yttrium oxyfluoride precursor; S3, mixing the yttrium oxyfluoride precursor, second solvent, and binder to carry out ball milling, granulation, and calcination to obtain yttrium oxyfluoride spraying powder; the precipitant in the preparation method of this invention includes carbonate and / or bicarbonate, the raw materials are safe and environmentally friendly, the cost is low, the process is simple and efficient, and stable industrial production can be achieved.

[0032] The wet precipitation and fluorination reactions enable the raw materials to achieve uniform mixing at the ionic or molecular level. The precipitants, including carbonates and / or bicarbonates, exhibit low agglomeration, high specific surface area, and spherical morphology, which also facilitates a more uniform fluorination reaction, improves powder dispersibility, and enhances product uniformity, providing a good foundation for subsequent spray granulation. The resulting yttrium fluoride spray powder exhibits high purity, regular morphology, concentrated particle size distribution, good sphericity, small angle of repose, and excellent flowability. In the semiconductor field, it can significantly improve the density, bonding strength, and plasma etching resistance of plasma-sprayed coatings, making it valuable for applications in key components such as corrosion-resistant coatings and plasma chamber liners in semiconductor manufacturing equipment. Attached Figure Description

[0033] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0034] Figure 1 These are electron microscope images of the precursor filter cake from Example 1; Figure 2 These are electron microscope images of the yttrium fluoride spray powder from Example 1; Figure 3 These are electron microscope images of the precursor filter cake from Example 2; Figure 4 These are electron microscope images of the yttrium fluoride spray powder from Example 2; Figure 5 These are electron microscope images of the yttrium fluoride spray powder from Example 3; Figure 6 This is an electron microscope image of the yttrium fluoride spray powder of Comparative Example 1; Figure 7 This is a particle size distribution image of the yttrium fluoride spraying powder from Example 1; Figure 8 This is an XRD image of the yttrium fluoride spray powder from Example 1. Detailed Implementation

[0035] The following embodiments are provided to better understand the present invention and are not limited to the preferred embodiments described. They do not constitute a limitation on the content and scope of protection of the present invention. Any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the protection scope of the present invention.

[0036] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains; the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the invention; the terms “comprising” and “having” and any variations thereof in the text of this invention are intended to cover non-exclusive inclusion.

[0037] In the description of the embodiments of the present invention, the technical terms "first", "second", etc. are used only to distinguish different objects and should not be construed as indicating or implying relative importance or implicitly indicating the number, specific order or primary and secondary relationship of the indicated technical features.

[0038] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of the invention. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.

[0039] The "range" disclosed in this invention is defined by a lower limit and an upper limit. A given range is defined by selecting a lower limit and an upper limit, which define the boundaries of the specific range. This range can include or exclude endpoints and can be arbitrarily combined; that is, any lower limit can be combined with any upper limit to form a range. In this invention, unless otherwise stated, the numerical range "ab" represents a shortened representation of any combination of real numbers from a to b, where a and b are real numbers. For example, the numerical range "0-5" indicates that all real numbers between "0-5" have been listed herein; "0-5" is merely a shortened representation of these numerical combinations. Furthermore, when a parameter is described as an integer ≥ 2, it is equivalent to disclosing that the parameter can be, for example, an integer 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0040] In the description of the embodiments of the present invention, the term "and / or" is merely a description of the relationship between associated objects, indicating that there can be three relationships. For example, A and / or B can represent three situations: A exists alone, A and B exist simultaneously, and B exists alone.

[0041] In the description of the embodiments of the present invention, the term "at least one" refers to one or more (including two).

[0042] For experiments not specifically described in the examples, the procedures or conditions should be followed according to the conventional experimental procedures described in the literature in this field. Reagents or instruments whose manufacturers are not specified are all commercially available conventional reagent products.

[0043] Example 1 This embodiment provides a yttrium fluoride oxyfluoride spraying powder, the preparation method of which includes the following steps: S1. Based on the mass ratio of yttrium in polyethylene glycol 2000 to yttrium oxide (converted to yttrium oxide) of yttrium nitrate (converted to yttrium oxide) of 1:100, yttrium nitrate, 100g of polyethylene glycol 2000, and water were mixed to obtain a mixed solution with a yttrium nitrate concentration of 0.5mol / L. According to the molar ratio of bicarbonate ions in ammonium bicarbonate to yttrium ions in yttrium nitrate of 3:1, the required amount of ammonium bicarbonate was weighed and dissolved in water to prepare an ammonium bicarbonate solution with a concentration of 2mol / L. At 25℃, the prepared ammonium bicarbonate solution was slowly added to the mixed solution over 1 hour to induce precipitation. After precipitation, the mixture was stirred and aged for 10 minutes, then filtered and washed with 1L of deionized water to obtain a precursor filter cake. The dried filter cake was shown in the electron micrograph. Figure 1 As shown in the figure, the yttrium carbonate precursor has a near-spherical morphology with low agglomeration, which is beneficial for the subsequent spray spheroidization process. The filter cake was then redispersed in water at a mass ratio of 1:2 to obtain a slurry. S2, ammonium fluoride and water are mixed to prepare an ammonium fluoride solution with a concentration of 2 mol / L. The required amount of ammonium fluoride solution is weighed according to the stoichiometric ratio of the target yttrium fluoride oxyfluoride, so that the molar ratio of fluoride ions in the ammonium fluoride solution to yttrium ions in the slurry is 1:1. The temperature is controlled at 50℃. Within 2 hours, the weighed ammonium fluoride solution is added to the slurry to carry out the fluorination reaction. After the fluorination is completed, the mixture is stirred and aged for 1 hour. Then it is filtered, washed with 1 L of deionized water, and dried at 60℃ for 24 hours to obtain the yttrium fluoride oxyfluoride precursor. S3, 5 kg of the yttrium oxyfluoride precursor obtained in step S2 was added to a ball mill, along with 7 kg of water and 50 g of carboxymethyl cellulose (1 wt% of the yttrium oxyfluoride precursor mass). The mixture was ball-milled at a ball-to-yttrium oxyfluoride precursor mass ratio of 4:1 at 500 rpm until the slurry D50 was below 1 μm. Spray granulation was then performed at an atomizer speed of 16500 rpm, an inlet temperature of 250℃, an outlet temperature of 120℃, and a material pumping speed controlled at 30 rpm. Calcination was carried out in an air atmosphere, with the temperature increased to 800℃ at a rate of 5℃ / min and held for 3 hours to obtain yttrium oxyfluoride spray powder. Electron micrographs are shown below. Figure 2 As shown in the figure, the sprayed powder has high sphericity, a smooth surface, and a uniform particle size distribution.

[0044] Example 2 This embodiment provides a yttrium fluoride oxyfluoride spraying powder, prepared according to the method of Example 1, except that in step S1, ammonium bicarbonate is replaced with sodium carbonate, and the powder is washed with water until the sodium ion impurities in the filtrate are below 100 ppm (ICP test). Electron micrographs of the dried filter cake are shown below. Figure 3 As shown in the image, the yttrium carbonate precursor has a spherical morphology, but exhibits uneven particle distribution and agglomeration; the obtained electron micrograph of the yttrium oxyfluoride sprayed powder is shown in the image. Figure 4As shown in the figure, it can be seen that the sphericity of the sprayed powder is slightly lower than that of Example 1, but the overall sphericity still meets the spraying requirements.

[0045] Example 3 This embodiment provides a yttrium fluoride oxyfluoride spraying powder, prepared according to the method of Example 1, except that in step S2, ammonium fluoride is replaced with trifluoroacetic acid. The resulting yttrium fluoride oxyfluoride spraying powder electron microscope image is shown below. Figure 5 As shown in the figure, the surface of the sprayed powder particles is slightly rough, but the spherical shape is well maintained.

[0046] Example 4 This embodiment provides a yttrium fluoride spraying powder, which is prepared in accordance with the method of Example 1. The difference is that in step S2, the amount of ammonium fluoride solution is adjusted so that the molar ratio of fluoride ions in the ammonium fluoride solution to yttrium ions in the yttrium carbonate slurry is 7:5.

[0047] Comparative Example 1 This comparative example provides a yttrium fluoride oxychloride spray powder, prepared according to the method of Example 1, except that in step S1, ammonium bicarbonate is replaced with oxalic acid. The resulting yttrium fluoride oxychloride spray powder electron microscope image is shown below. Figure 6 As shown in the figure, it can be seen that the powder particles in Comparative Example 1 have irregular shapes and contain many fragments and adhesions.

[0048] Test case The yttrium fluoride spray powders prepared in the examples and comparative examples were tested. Morphology: Tested using a Hitachi scanning electron microscope (Japan); Phase composition: Measured using a Bruker X-ray diffractometer (Germany); Particle size (D10, D50, D90): tested using a domestic Omec laser particle size analyzer; Sphericity: Tested using a powder angle of repose measuring instrument, the test method conforms to the national standard GB / T16913; Loose packing density: Tested using a natural bulk density meter, and the test method conforms to the national standard GB / T16913; Test data are shown in Table 1; Table 1. Particle size and bulk characteristics of yttrium fluoride spray powder

[0049] The particle size distribution image of the yttrium fluoride spraying powder provided in Example 1 is shown below. Figure 7 The figure shows that the particle size distribution is concentrated and symmetrical with a single peak; the XRD of Example 1 is as follows. Figure 8 The diffraction peaks in the figure are consistent with the standard yttrium fluoride (YOF) spectrum, and there are no impurities, indicating that the product has high purity.

[0050] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A method for preparing yttrium fluoride spraying powder, characterized in that, The preparation method includes the following steps: S1, a soluble yttrium salt, dispersant, first solvent, and precipitant are mixed and subjected to a precipitation reaction to obtain a slurry; The precipitant includes carbonates and / or bicarbonates; S2, the slurry and fluorinating agent are mixed and fluorinated to obtain the yttrium oxyfluoride precursor; S3, the yttrium oxyfluoride precursor, the second solvent, and the binder are mixed, ball-milled, granulated, and calcined to obtain yttrium oxyfluoride spray powder.

2. The preparation method according to claim 1, characterized in that, The soluble yttrium salts include inorganic soluble yttrium salts; And / or, the dispersant includes an organic dispersant; And / or, the ratio of the mass of the dispersant to the mass of yttrium in the soluble yttrium salt converted to yttrium oxide is (0.1-3):100; And / or, the molar ratio of carbonate ions and / or bicarbonate ions in the precipitant to yttrium ions in the soluble yttrium salt is (1-6):1; And / or, the precipitant includes at least one of sodium carbonate, potassium carbonate, ammonium carbonate, sodium bicarbonate, potassium bicarbonate, and ammonium bicarbonate.

3. The preparation method according to claim 2, characterized in that, The soluble yttrium salt includes at least one of yttrium chloride, yttrium acetate, and yttrium nitrate; And / or, the dispersant includes at least one of polyethylene glycol, stearic acid, and oleic acid; And / or, the molar ratio of carbonate ions and / or bicarbonate ions in the precipitant to yttrium ions in the soluble yttrium salt is (2-4):1; And / or, the precipitant includes ammonium carbonate and / or ammonium bicarbonate.

4. The preparation method according to claim 1, characterized in that, The molar ratio of fluoride ions in the fluorinating agent to yttrium ions in the slurry is (1-2.5):1; And / or, the fluorinating agent includes fluorinated organic carboxylic acids and / or fluorinated salts.

5. The preparation method according to claim 4, characterized in that, The molar ratio of fluoride ions in the fluorinating agent to yttrium ions in the slurry is (1-1.2):1; And / or, the fluorinating agent includes at least one of trifluoroacetic acid, ammonium fluoride, sodium fluoride, and potassium fluoride.

6. The preparation method according to claim 1, characterized in that, The mass ratio of the yttrium oxyfluoride precursor to the second solvent is (1-6):(4-7); And / or, the amount of the binder is 0.1-3 wt% based on the mass of the yttrium oxyfluoride precursor.

7. The preparation method according to claim 1, characterized in that, The ball mill rotates at 300-600 rpm and grinds until the slurry D50 is below 1 μm; And / or, the granulation rotation speed is 13000-26000 rpm, the inlet temperature is 200-300℃, the outlet temperature is 100-200℃, and the material pumping speed is 25-50 rpm. And / or, the granulation process yields particles with a D50 of 15-70 μm and a (D90-D10) / 2×D50 of 0.2-0.

7. And / or, the calcination heating rate is 1-5℃ / min, the temperature is 500-1200℃, and the time is 3-10h.

8. The preparation method according to claim 1, characterized in that, In step S1, the precipitation reaction is carried out at a temperature of 25-60℃ for 0.5-3 hours. And / or, in step S2, the fluorination reaction is carried out at a temperature of 25-60°C for a time of 0.5-2 hours.

9. A yttrium fluoride spraying powder prepared by the preparation method according to any one of claims 1-8.

10. The application of the yttrium fluoride spraying powder according to claim 9 in the semiconductor field.

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