Sample preparation method for particle size detection of high-purity titanium powder and application thereof

Abstract

The application provides a sample preparation method for particle size detection of high-purity titanium powder and application thereof. The sample preparation method comprises the following steps: (1) mixing high-purity titanium powder and a first acid to perform a first reaction, adding a second acid after the reaction is completed, performing a second reaction, and obtaining a reaction product; and (2) mixing the reaction product and a dissolving agent, and then constant volume to obtain a sample preparation solution. The sample preparation method provided by the application can not only ensure that no pollution is introduced in the sample preparation process, make the detection result truly reflect the particle size distribution of the titanium powder, and improve the accuracy of the particle size detection, but also has high stability and high efficiency, can complete the sample preparation in a short time, and improve the detection efficiency. Moreover, the sample preparation method has strong operability, high safety, reduces the difficulty and cost of sample preparation, and is convenient for popularization and application.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of analytical testing, and particularly relates to a sample preparation method for particle size detection of high-purity titanium powder and application thereof. BACKGROUND

[0002] A liquid particle counter (LPC) is a device for detecting the number and size distribution of particles suspended in a liquid. The KS-42C detector of Rion can detect the number of particles within 0.5-20 microns, and is provided with a maximum of 10 detection channels. It adopts the light scattering principle: when a light beam is directed at particles suspended in a liquid, part of the light is absorbed, and another part of the light is scattered; by measuring the change of scattered light intensity with scattering angle, the size and distribution of particles can be determined.

[0003] High-purity titanium powder is a metal powder made of titanium, which is a silver-gray irregular powder with high air absorption capacity and easy to burn under high temperature or electric spark conditions. Titanium powder is an important raw material for powder metallurgy, alloy material additive, metal ceramic, surface coating agent, aluminum alloy additive, electric vacuum air adsorber, spraying and plating, and is also applied to aerospace, spraying metallurgy, fireworks and other industries. Titanium powder is more active than metal titanium, and is more likely to react with other elements or compounds, and is more likely to oxidize, burn and explode, which belongs to dangerous goods. The shape of powder particles is determined by the powder industry, and different particle shapes have a great influence on the performance of powder metallurgy process, which directly affects the strength of the product. The specific surface area of powder particles directly affects the pressing and sintering performance of the powder. Naturally, the specific surface area of titanium powder with larger specific surface area has better pressing and sintering performance. The specific surface area of powder is related to particle size, shape and external shape. The finer the powder particle size, the more complex the shape, and the rougher the external surface, the larger the specific surface area of the particle, and vice versa.

[0004] In the prior art, the means for detecting the number and size distribution of particles insoluble in acid in high-purity titanium powder will introduce pollution in the sample preparation process, and the accuracy of the detection result is deviated.

[0005] Therefore, how to effectively avoid the pollution of high-purity titanium powder in the sample preparation process and improve the accuracy of particle size detection is a technical problem to be solved. SUMMARY

[0006] In view of the deficiencies of the prior art, the purpose of the present application is to provide a sample preparation method for particle size detection of high-purity titanium powder and application thereof. The sample preparation method provided by the present application can not only ensure that no pollution is introduced in the sample preparation process, so that the detection result truly reflects the particle size distribution of titanium powder and improves the accuracy of particle size detection, but also has high stability and high efficiency, and can complete sample preparation in a short time and improve detection efficiency. Moreover, the sample preparation method has strong operability, high safety, reduces the difficulty and cost of sample preparation, and is convenient for popularization and application.

[0007] To achieve the object of the present application, the present application adopts the following technical solutions:

[0008] In a first aspect, the present application provides a sample preparation method for particle size detection of high-purity titanium powder, which comprises the following steps:

[0009] (1) mixing high-purity titanium powder and a first acid to perform a first reaction, adding a second acid after the reaction is completed, performing a second reaction, and obtaining a reaction product.

[0010] (2) mixing the reaction product and a dissolving agent, and then making up the volume to obtain a sample preparation solution.

[0011] The sample preparation method provided by the present application not only ensures that no contamination is introduced during the sample preparation process, but also makes the detection result truly reflect the particle size distribution of the titanium powder, thereby improving the accuracy of the particle size detection. Moreover, the sample preparation method has high stability and high efficiency, and can complete the sample preparation in a short time, thereby improving the detection efficiency. Furthermore, the sample preparation method has strong operability, high safety, and reduces the difficulty and cost of sample preparation, thereby facilitating popularization and application.

[0012] Preferably, the purity of the high-purity titanium powder in step (1) is ≥ 99.5%, for example, it can be 99.5%, 99.6%, 99.7%, 99.8%, or 99.9%, etc.

[0013] Preferably, the mass-to-volume ratio of the high-purity titanium powder and the first acid in step (1) is 0.5 g:(2-8) mL, for example, it can be 0.5 g:2 mL, 0.5 g:3 mL, 0.5 g:4 mL, 0.5 g:5 mL, 0.5 g:6 mL, 0.5 g:7 mL, or 0.5 g:8 mL, etc.

[0014] In the present application, using a suitable mass-to-volume ratio of high-purity titanium powder and first acid helps to ensure stable reaction rate and full reaction of high-purity titanium powder, and helps to maintain the uniformity of the reaction system and avoid excessive local reaction concentration differences.

[0015] Preferably, the first acid in step (1) comprises hydrofluoric acid.

[0016] Preferably, the concentration of the first acid in step (1) is 30-50 wt%, for example, it can be 30 wt%, 40 wt%, or 50 wt%, etc.

[0017] In the present application, this concentration range can not only ensure that the reaction has a suitable rate, allowing the metal to gradually dissolve and participate in the reaction to generate corresponding fluoride products, but also facilitate subsequent processing and regulation of the reaction system.

[0018] Preferably, the temperature of the first reaction in step (1) is 40-80℃, for example, it can be 40℃, 50℃, 60℃, 70℃, or 80℃, etc.

[0019] In this invention, a suitable reaction temperature accelerates molecular motion, allowing hydrofluoric acid molecules to come into contact with titanium powder particles more frequently. This also helps to break down the protective oxide film on the titanium surface, promoting a sustained and efficient reaction. However, excessively high temperatures exacerbate hydrofluoric acid volatilization, leading not only to material loss but also to a deterioration of the operating environment, posing serious safety and health hazards.

[0020] Preferably, the reaction time in step (1) is 0.5-1.5h, for example, it can be 0.5h, 1h or 1.5h.

[0021] Preferably, in step (1), the second acid includes hydrofluoric acid.

[0022] Preferably, in step (1), the concentration of the second acid is 15-25 wt%, for example, it can be 15 wt%, 20 wt%, or 25 wt%.

[0023] In this invention, a suitable concentration of the second acid helps to ensure that the titanium powder reacts completely, and that the reaction proceeds smoothly and the process is controllable.

[0024] Preferably, in step (2), the volume ratio of the first acid and the second acid is (4-6):(6-4), wherein the first acid is selected from the range "4-6", which can be, for example, 4, 5 or 6, and the second acid is selected from the range "6-4", which can be, for example, 4, 5 or 6.

[0025] In this invention, a suitable volume ratio of the first acid and the second acid helps to fully react all the titanium powder.

[0026] Preferably, the temperature of the second reaction in step (1) is 20-30°C, for example, it can be 20°C, 25°C or 30°C.

[0027] Within this temperature range, the reaction rate is relatively moderate. It avoids the problem of excessively low temperatures leading to overly slow reactions and reduced production efficiency, while also preventing excessively high temperatures from causing uncontrollable reactions. This ensures relatively high safety, and the reaction temperature of 20-30°C helps generate relatively stable products. Taking titanium tetrafluoride, produced by the reaction of titanium powder with hydrofluoric acid, as an example, its chemical properties are relatively stable at this temperature, making it less prone to further decomposition or other side reactions. This improves the quality and purity of the product, facilitating subsequent applications.

[0028] Preferably, the reaction time in step (2) is 3-8 minutes, for example, 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes or 8 minutes.

[0029] Preferably, the solvent in step (2) includes nitric acid.

[0030] Preferably, the volume ratio of the reaction product to the solvent in step (2) is 10:(0.8-1.2), for example, it can be 10:0.8, 10:0.9, 10:1, 10:1.1 or 10:1.2, etc.

[0031] In this invention, nitric acid has strong oxidizing properties, which can convert the reaction products into more soluble high-valence compounds, thereby accelerating the dissolution rate. An appropriate content can make the dissolution process more efficient and thorough, while ensuring the chemical stability of each substance in the solution, which is beneficial for subsequent processing and analysis of the solution.

[0032] Preferably, the sample preparation method includes the following steps:

[0033] Place high-purity titanium powder with a purity ≥ 99.5% in a beaker, then slowly add the first acid dropwise. The mass-to-volume ratio of high-purity titanium powder to the first acid is 0.5 g:(2-8) mL. After the first reaction is carried out at 40-80℃ for 0.5-1.5 h, add the second acid dropwise at 20-30℃. The volume ratio of the first acid to the second acid is (4-6):(6-4). Carry out the second reaction for 3-8 min. After the reaction is completed, add the solvent dropwise to the reaction product. The volume ratio of the reaction product to the solvent is 10:(0.8-1.2). Then transfer the obtained solution to a volumetric flask, add water (e.g., ultrapure water) to make up to the final volume, and obtain the sample preparation solution.

[0034] Secondly, the present invention provides an application of a sample preparation solution prepared by the sample preparation method described in the first aspect in particle size detection.

[0035] Preferably, the application steps of the sample preparation solution in particle size detection include:

[0036] The liquid particle counter is pretreated, and then the sampling tube of the liquid particle counter is inserted into the sample solution for detection. The detection is performed multiple times and the average value is taken to obtain the detection result.

[0037] Preferably, the preprocessing step includes:

[0038] Take clean electronic-grade ultrapure water (i.e., pure water with a resistivity of 18MΩ), test it in a liquid particle counter, clean the pipeline and verify whether the pure water meets the standard. If the pure water data is within the specification range, the subsequent steps can be carried out.

[0039] The numerical range described in this invention includes not only the point values ​​listed above, but also any point values ​​within the numerical ranges not listed above. Due to space limitations and for the sake of brevity, this invention will not exhaustively list all the specific point values ​​included in the range.

[0040] Compared with the prior art, the present invention has the following beneficial effects:

[0041] The sample preparation method provided by this invention not only ensures that no contamination is introduced during the sample preparation process, allowing the test results to truly reflect the particle size distribution of titanium powder and improving the accuracy of particle size detection, but also exhibits high stability and efficiency, enabling sample preparation to be completed in a short time and improving detection efficiency. Furthermore, this sample preparation method is highly operable and safe, reducing the difficulty and cost of sample preparation and facilitating its widespread application. Attached Figure Description

[0042] Figure 1 This is a flow chart of the sample preparation process for particle size detection of high-purity titanium powder provided in Embodiment 1 of the present invention. Detailed Implementation

[0043] The technical solution of the present invention will be further illustrated below through specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be construed as limiting the invention in any way.

[0044] It should be noted that the purity of the high-purity titanium powder mentioned in the following embodiments is 99.9%.

[0045] Example 1

[0046] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, and its process flow diagram is shown below. Figure 1 As shown, the sample preparation method includes the following steps:

[0047] 0.5g of high-purity titanium powder was placed in a polytetrafluoroethylene beaker, and then 5mL of the first acid (i.e., 40wt% hydrofluoric acid) was slowly added dropwise. The mass-volume ratio of high-purity titanium powder to the first acid was 0.5g:5mL. After the first reaction was carried out at 60℃ for 1h, 5mL of the second acid (i.e., 20wt% hydrofluoric acid) was added at 25℃. The volume ratio of the first acid to the second acid was 5:5. The mixture was allowed to stand for 5min to carry out the second reaction. After the reaction was completed, 1mL of solvent (i.e., nitric acid) was added dropwise to the reaction product. The volume ratio of the reaction product to the solvent was 10:1. The resulting solution was then transferred to a volumetric flask, and ultrapure water was added to make up to 100mL to obtain the sample preparation solution.

[0048] Example 2

[0049] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method including the following steps:

[0050] 0.5 g of high-purity titanium powder was placed in a polytetrafluoroethylene beaker, and then 4 mL of the first acid (i.e., 50 wt% hydrofluoric acid) was slowly added dropwise. The mass-volume ratio of high-purity titanium powder to the first acid was 0.5 g: 3 mL. After the first reaction was carried out at 40 °C for 1.5 h, 6 mL of the second acid (i.e., 25 wt% hydrofluoric acid) was added at 20 °C. The volume ratio of the first acid to the second acid was 4:6. The mixture was allowed to stand for 3 min for the second reaction. After the reaction was completed, 0.8 mL of solvent (i.e., nitric acid) was added dropwise to the reaction product. The volume ratio of the reaction product to the solvent was 10:0.8. The resulting solution was then transferred to a volumetric flask, and ultrapure water was added to bring the volume to 100 mL to obtain the sample preparation solution.

[0051] Example 3

[0052] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method including the following steps:

[0053] 0.5 g of high-purity titanium powder was placed in a polytetrafluoroethylene beaker, and then 6 mL of the first acid (i.e., 30 wt% hydrofluoric acid) was slowly added dropwise. The mass-volume ratio of high-purity titanium powder to the first acid was 0.5 g: 6 mL. After the first reaction was carried out at 80 °C for 0.5 h, 4 mL of the second acid (i.e., 15 wt% hydrofluoric acid) was added at 30 °C. The volume ratio of the first acid to the second acid was 6:4. The mixture was allowed to stand for 8 min for the second reaction. After the reaction was completed, 1.2 mL of solvent (i.e., nitric acid) was added dropwise to the reaction product. The volume ratio of the reaction product to the solvent was 10:1.2. The resulting solution was then transferred to a volumetric flask, and ultrapure water was added to bring the volume to 100 mL to obtain the sample preparation solution.

[0054] Example 6

[0055] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method including the following steps:

[0056] 0.5g of high-purity titanium powder was placed in a polytetrafluoroethylene beaker, and then 5mL of the first acid (i.e., 40wt% hydrofluoric acid) was slowly added dropwise. The mass-volume ratio of high-purity titanium powder to the first acid was 0.5g:1mL. After the first reaction was carried out at 60℃ for 1h, 5mL of the second acid (i.e., 20wt% hydrofluoric acid) was added at 25℃. The volume ratio of the first acid to the second acid was 5:5. The mixture was allowed to stand for 5min to carry out the second reaction. After the reaction was completed, 1mL of solvent (i.e., nitric acid) was added dropwise to the reaction product. The volume ratio of the reaction product to the solvent was 10:1. The resulting solution was then transferred to a volumetric flask, and ultrapure water was added to make up to 100mL to obtain the sample preparation solution.

[0057] Example 7

[0058] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method including the following steps:

[0059] Place 0.5g of high-purity titanium powder in a polytetrafluoroethylene beaker, then slowly add 5mL of the first acid (i.e., 40wt% hydrofluoric acid). The mass-volume ratio of high-purity titanium powder to the first acid is 0.5g:10mL. After the first reaction is carried out at 60℃ for 1h, add 5mL of the second acid (i.e., 20wt% hydrofluoric acid) at 25℃. The volume ratio of the first acid to the second acid is 5:5. Let stand for 5min to carry out the second reaction. After the reaction is completed, add 1mL of solvent (i.e., nitric acid) to the reaction product. The volume ratio of the reaction product to the solvent is 10:1. Then transfer the obtained solution to a volumetric flask, add ultrapure water to make up to 100mL, and obtain the sample preparation solution.

[0060] Example 8

[0061] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method including the following steps:

[0062] Place 0.5g of high-purity titanium powder in a polytetrafluoroethylene beaker, then slowly add 5mL of the first acid (i.e., 40wt% hydrofluoric acid). The mass-volume ratio of high-purity titanium powder to the first acid is 0.5g:5mL. After the first reaction is carried out at 30℃ for 1h, add 5mL of the second acid (i.e., 20wt% hydrofluoric acid) at 25℃. The volume ratio of the first acid to the second acid is 5:5. Let stand for 5min to carry out the second reaction. After the reaction is completed, add 1mL of solvent (i.e., nitric acid) to the reaction product. The volume ratio of the reaction product to the solvent is 10:1. Then transfer the obtained solution to a volumetric flask, add ultrapure water to make up to 100mL, and obtain the sample preparation solution.

[0063] Example 9

[0064] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method including the following steps:

[0065] 0.5g of high-purity titanium powder was placed in a polytetrafluoroethylene beaker, and then 5mL of the first acid (i.e., 40wt% hydrofluoric acid) was slowly added dropwise. The mass-volume ratio of high-purity titanium powder to the first acid was 0.5g:5mL. After the first reaction was carried out at 90℃ for 1h, 5mL of the second acid (i.e., 20wt% hydrofluoric acid) was added at 25℃. The volume ratio of the first acid to the second acid was 5:5. The mixture was allowed to stand for 5min to carry out the second reaction. After the reaction was completed, 1mL of solvent (i.e., nitric acid) was added dropwise to the reaction product. The volume ratio of the reaction product to the solvent was 10:1. The resulting solution was then transferred to a volumetric flask, and ultrapure water was added to make up to 100mL to obtain the sample preparation solution.

[0066] Example 10

[0067] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method including the following steps:

[0068] Place 0.5g of high-purity titanium powder in a polytetrafluoroethylene beaker, then slowly add 5mL of the first acid (i.e., 40wt% hydrofluoric acid). The mass-volume ratio of high-purity titanium powder to the first acid is 0.5g:5mL. After the first reaction is carried out at 60℃ for 1h, add 10mL of the second acid (i.e., 20wt% hydrofluoric acid) at 25℃. The volume ratio of the first acid to the second acid is 5:10. Let stand for 5min to carry out the second reaction. After the reaction is completed, add 1mL of solvent (i.e., nitric acid) to the reaction product. The volume ratio of the reaction product to the solvent is 10:1. Then transfer the obtained solution to a volumetric flask, add ultrapure water to make up to 100mL, and obtain the sample preparation solution.

[0069] Example 11

[0070] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method including the following steps:

[0071] 0.5g of high-purity titanium powder was placed in a polytetrafluoroethylene beaker, and then 5mL of the first acid (i.e., 40wt% hydrofluoric acid) was slowly added dropwise. The mass-volume ratio of high-purity titanium powder to the first acid was 0.5g:5mL. After the first reaction was carried out at 60℃ for 1h, 2.5mL of the second acid (i.e., 20wt% hydrofluoric acid) was added at 25℃. The volume ratio of the first acid to the second acid was 5:2.5. The mixture was allowed to stand for 5min to carry out the second reaction. After the reaction was completed, 1mL of solvent (i.e., nitric acid) was added dropwise to the reaction product. The volume ratio of the reaction product to the solvent was 10:1. The resulting solution was then transferred to a volumetric flask, and ultrapure water was added to make up to 100mL to obtain the sample preparation solution.

[0072] Example 12

[0073] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method including the following steps:

[0074] 0.5g of high-purity titanium powder was placed in a polytetrafluoroethylene beaker, and then 5mL of the first acid (i.e., 40wt% hydrofluoric acid) was slowly added dropwise. The mass-volume ratio of high-purity titanium powder to the first acid was 0.5g:5mL. After the first reaction was carried out at 60℃ for 1h, 5mL of the second acid (i.e., 20wt% hydrofluoric acid) was added at 15℃. The volume ratio of the first acid to the second acid was 5:5. The mixture was allowed to stand for 5min to carry out the second reaction. After the reaction was completed, 1mL of solvent (i.e., nitric acid) was added dropwise to the reaction product. The volume ratio of the reaction product to the solvent was 10:1. The resulting solution was then transferred to a volumetric flask, and ultrapure water was added to make up to 100mL to obtain the sample preparation solution.

[0075] Example 13

[0076] This embodiment provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method including the following steps:

[0077] 0.5g of high-purity titanium powder was placed in a polytetrafluoroethylene beaker, and then 5mL of the first acid (i.e., 40wt% hydrofluoric acid) was slowly added dropwise. The mass-volume ratio of high-purity titanium powder to the first acid was 0.5g:5mL. After the first reaction was carried out at 60℃ for 1h, 5mL of the second acid (i.e., 20wt% hydrofluoric acid) was added at 40℃. The volume ratio of the first acid to the second acid was 5:5. The mixture was allowed to stand for 5min to carry out the second reaction. After the reaction was completed, 1mL of solvent (i.e., nitric acid) was added dropwise to the reaction product. The volume ratio of the reaction product to the solvent was 10:1. The resulting solution was then transferred to a volumetric flask, and ultrapure water was added to make up to 100mL to obtain the sample preparation solution.

[0078] Example 14

[0079] The difference between this embodiment and Embodiment 1 is that the first acid is hydrofluoric acid with a concentration of 20 wt%.

[0080] The remaining sample preparation methods and parameters are consistent with those in Example 1.

[0081] Example 15

[0082] The difference between this embodiment and Embodiment 1 is that the second acid is hydrofluoric acid with a concentration of 40 wt%.

[0083] The remaining sample preparation methods and parameters are consistent with those in Example 1.

[0084] Comparative Example 1

[0085] This comparative example provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method comprising the following steps:

[0086] Place 0.5g of high-purity titanium powder in a polytetrafluoroethylene beaker, and then slowly add 5mL of the first acid (i.e., 40wt% hydrofluoric acid). The mass-volume ratio of high-purity titanium powder to the first acid is 0.5g:5mL. The first reaction is carried out at 60℃ for 1h. After the reaction is completed, add 1mL of solvent (i.e., nitric acid) to the reaction product. The volume ratio of the reaction product to the solvent is 10:1. Then transfer the obtained solution to a volumetric flask, add ultrapure water to make up to 100mL, and obtain the sample preparation solution.

[0087] Comparative Example 2

[0088] This comparative example provides a sample preparation method for high-purity titanium powder used in particle size detection, the sample preparation method comprising the following steps:

[0089] Place 0.5g of high-purity titanium powder in a polytetrafluoroethylene beaker, then add 5mL of a second acid (i.e., 20wt% hydrofluoric acid) at 25℃, let stand for 5min to carry out the second reaction, and after the reaction is completed, add 1mL of solvent (i.e., nitric acid) dropwise to the reaction product. The volume ratio of reaction product to solvent is 10:1. Then transfer the obtained solution to a volumetric flask, add ultrapure water to make up to 100mL, and obtain the sample preparation solution.

[0090] Performance testing

[0091] The particle size of the sample solutions provided in the above embodiments and comparative examples was measured to calculate the standard deviation. The specific steps included:

[0092] (a) Take clean electronic-grade ultrapure water (i.e., pure water with a resistivity of 18 MΩ), test it in a liquid particle counter, clean the pipeline and verify whether the pure water meets the standard. If the pure water data is within the specification range, the subsequent steps can be carried out.

[0093] (b) Insert the sampling tube of the liquid particle counter into the sample preparation solution, rinse the tube three times with 10 mL each time, and then perform three tests, each test requiring 10 mL of solution.

[0094] (c) The standard deviation was calculated by performing three particle counts of high-purity titanium powder.

[0095] The results are shown in Table 1.

[0096] Table 1

[0097]

[0098]

[0099] analyze:

[0100] As shown in the table above, the sample preparation method provided by this invention not only ensures that no contamination is introduced during the sample preparation process, allowing the test results to truly reflect the particle size distribution of titanium powder and improving the accuracy of particle size detection, but also exhibits high stability and efficiency, enabling sample preparation to be completed in a short time and improving detection efficiency. Furthermore, this sample preparation method is highly operable and safe, reducing the difficulty and cost of sample preparation and facilitating its widespread application.

[0101] The applicant declares that the present invention is illustrated by the above embodiments, but the present invention is not limited to the above process steps, that is, it does not mean that the present invention must rely on the above process steps to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions of the raw materials used in the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A sample preparation method for high-purity titanium powder used in particle size detection, characterized in that, The sample preparation method includes the following steps: (1) Mix high-purity titanium powder with a purity of ≥99.5% with the first acid to carry out the first reaction. After the reaction is completed, add the second acid to carry out the second reaction to obtain the reaction product; Step (1) The concentration of the first acid is 30-50 wt%; Step (1) The concentration of the second acid is 15-25 wt%; Step (1) The first acid includes hydrofluoric acid; Step (1) The second acid includes hydrofluoric acid; Step (1) The mass-volume ratio of the high-purity titanium powder and the first acid is 0.5 g:(2-8) mL; Step (1) The volume ratio of the first acid and the second acid is (4-6):(6-4); In step (1), the temperature of the first reaction is 40-80℃; in step (1), the time of the first reaction is 0.5-1.5h; in step (1), the temperature of the second reaction is 20-30℃; and the time of the second reaction is 3-8min. (2) The reaction product and the solvent are mixed and then the volume is adjusted to obtain the sample preparation solution; the solvent in step (2) includes nitric acid; the volume ratio of the reaction product and the solvent in step (2) is 10:(0.8-1.2).

2. The application of a sample preparation solution prepared by the sample preparation method as described in claim 1 in particle size detection.

3. The application according to claim 2, characterized in that, The steps for applying the sample preparation solution in particle size detection include: The liquid particle counter is pretreated, and then the sampling tube of the liquid particle counter is inserted into the sample solution for detection. The detection is performed multiple times and the average value is taken to obtain the detection result.

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