Sample preparation method for granularity detection of high-purity titanium powder and application of sample preparation method

Abstract

The invention provides a sample preparation method for granularity detection of high-purity titanium powder and application of the sample preparation method. The sample preparation method comprises the following steps: preparing a sample; the method comprises the following steps: (1) mixing high-purity titanium powder with first acid, carrying out first reaction, adding second acid after the reaction is finished, and carrying out second reaction to obtain a reaction product; and (2) mixing the reaction product with a dissolving agent, and then fixing the volume to obtain a sample preparation solution. The sample preparation method provided by the invention not only can ensure that pollution is not introduced in the sample preparation process, so that the detection result truly reflects the particle size distribution of the titanium powder, and the particle size detection accuracy is improved, but also has high stability and high efficiency, can complete sample preparation within a relatively short time, and improves the detection efficiency. Moreover, the sample preparation method is high in operability and safety, the sample preparation difficulty and cost are reduced, and popularization and application are facilitated.

Description

Technical Field

[0001] The invention belongs to the technical field of analysis and testing, and specifically relates to a sample preparation method for particle size detection of high-purity titanium powder and application thereof. Background Art

[0002] Liquid particle counter (LPC) is a device that detects the number of suspended particles in liquid and the distribution of particle sizes. Liyin's KS-42C detector can detect the number of particles within 0.5-20μm, with up to 10 detection channels. It uses the principle of light scattering: when a light beam is directed to particles suspended in a liquid, part of the light is absorbed and the other part is scattered; by measuring the change in scattered light intensity with the scattering angle, the size of the particles and their distribution can be determined.

[0003] High-purity titanium powder is a metal powder made of titanium. It is a silver-grey irregular powder with a large air absorption capacity and is flammable under high temperature or electric spark conditions. Titanium powder is an additive for powder metallurgy and alloy materials. It is also an important raw material for metal ceramics, surface coating agents, aluminum alloy additives, electric vacuum getters, spraying, plating, etc. It is also used in aerospace, spray metallurgy, fireworks and other industries. Titanium powder is more active than metal titanium, and is more likely to react with other elements or compounds. It is more oxidizable, flammable, and explosive, and is a dangerous item. The shape of the powder particles is determined by the powder making industry. Different particle shapes have a great influence on the performance of the powder metallurgy process and directly affect the strength of the product. The specific surface area of ​​the powder particles directly affects the pressing and sintering properties of the powder. Naturally, the pressing and sintering properties of titanium powder with a large specific surface are better. The specific surface area of ​​the powder is related to the particle size, shape and appearance of the particles. The finer the powder particle size, the more complex the shape, and the rougher and more porous the appearance, the larger the specific surface area of ​​the particles, and vice versa.

[0004] In the prior art, the means of detecting the number and size distribution of acid-insoluble particles in high-purity titanium powder may cause contamination during the sample preparation process and the accuracy of the detection results may deviate.

[0005] Therefore, how to effectively avoid the contamination of high-purity titanium powder during the sample preparation process and improve the accuracy of particle size detection is a technical problem that needs to be solved urgently. Summary of the invention

[0006] In view of the deficiencies of the prior art, the object of the present invention is to provide a sample preparation method for particle size detection of high-purity titanium powder and its application. The sample preparation method provided by the present invention can not only ensure that no pollution is introduced during the sample preparation process, so that the detection results truly reflect the particle size distribution of titanium powder, and improve the accuracy of particle size detection, but also the sample preparation method has high stability and high efficiency, and can complete the sample preparation in a relatively short time, thereby improving the detection efficiency. In addition, the sample preparation method has strong operability and high safety, reduces the difficulty and cost of sample preparation, and is easy to promote and apply.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a method for preparing a sample of high-purity titanium powder for particle size detection, the method comprising the following steps:

[0009] (1) High-purity titanium powder and a first acid are mixed to carry out a first reaction, and after the reaction is completed, a second acid is added to carry out a second reaction to obtain a reaction product.

[0010] (2) The reaction product and a solvent are mixed, and then the volume is fixed to obtain a sample preparation solution.

[0011] The sample preparation method provided by the present invention can not only ensure that no pollution is introduced during 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 the sample preparation method has high stability and high efficiency, and can complete the sample preparation in a relatively short time, thereby improving the detection efficiency. In addition, the sample preparation method has strong operability and high safety, reduces the difficulty and cost of sample preparation, and is easy to promote and apply.

[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%.

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

[0014] In the present invention, using a suitable mass-to-volume ratio of high-purity titanium powder and the first acid helps to ensure a stable reaction rate and sufficient reaction of the high-purity titanium powder, helps to maintain the uniformity of the reaction system, and avoids excessive differences in local reactant concentrations.

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

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

[0017] In the present invention, 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 products such as fluoride, but also facilitate the subsequent treatment and regulation of the reaction system.

[0018] Preferably, the temperature of the first reaction in step (1) is 40-80°C, for example, 40°C, 50°C, 60°C, 70°C or 80°C.

[0019] In the present invention, a moderate reaction temperature can accelerate molecular motion, allowing hydrofluoric acid molecules to contact titanium powder particles more frequently, and also help to destroy the protective oxide film on the titanium surface, so as to promote the reaction to proceed continuously and efficiently. However, when the temperature is too high, the volatilization of hydrofluoric acid intensifies, which not only causes material loss, but also deteriorates the operating environment, bringing serious safety and health risks.

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

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

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

[0023] In the present invention, the second acid of appropriate concentration helps to make the titanium powder react completely, and the reaction proceeds smoothly and the process is controllable.

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

[0025] In the present invention, a suitable volume ratio of the first acid to 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, 20°C, 25°C or 30°C.

[0027] In this temperature range, the reaction rate of the present invention is relatively moderate, and the reaction will not be too slow due to too low a temperature, which affects the production efficiency, nor will the reaction be too violent and difficult to control due to too high a temperature. The safety is relatively high, and the reaction temperature of 20-30°C is conducive to the generation of relatively stable products. Taking titanium tetrafluoride generated by the reaction of titanium powder and hydrofluoric acid as an example, at this temperature, its chemical properties are relatively stable, and it is not easy to further decompose or other side reactions, which is conducive to improving the quality and purity of the product and is convenient for subsequent applications.

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

[0029] Preferably, the dissolving agent in step (2) comprises nitric acid.

[0030] Preferably, the volume ratio of the reaction product and the dissolving agent 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 the present invention, nitric acid has strong oxidizing properties and can convert the reaction products into more soluble high-valent compounds, thereby accelerating the dissolution rate. The 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 to the subsequent treatment and analysis of the solution.

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

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

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

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

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

[0037] Preferably, the pre-processing step comprises:

[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, proceed to the subsequent steps.

[0039] The numerical range described in the present invention not only includes the point values ​​listed above, but also includes any point values ​​between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists 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 the present invention can not only ensure that no pollution is introduced during 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 the sample preparation method has high stability and high efficiency, and can complete the sample preparation in a relatively short time, thereby improving the detection efficiency. In addition, the sample preparation method has strong operability and high safety, reduces the difficulty and cost of sample preparation, and is easy to promote and apply. BRIEF DESCRIPTION OF THE DRAWINGS

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

[0043] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[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 method for preparing a sample of high-purity titanium powder for particle size detection, and its process flow chart is as follows: Figure 1 As shown, the sample preparation method comprises the following steps:

[0047] Place 0.5 g of high-purity titanium powder in a polytetrafluoroethylene beaker, and then slowly add 5 mL of the first acid (i.e., hydrofluoric acid with a concentration of 40 wt%), the mass volume ratio of the high-purity titanium powder and the first acid is 0.5 g:5 mL. After a first reaction at 60°C for 1 hour, add 5 mL of the second acid (i.e., hydrofluoric acid with a concentration of 20 wt%) at 25°C, the volume ratio of the first acid to the second acid is 5:5, and let stand for 5 minutes for a second reaction. After the reaction is completed, add 1 mL of a solvent (i.e., nitric acid) to the reaction product, the volume ratio of the reaction product to the solvent is 10:1, and then transfer the obtained solution to a volumetric flask, add ultrapure water to make the volume up to 100 mL, and obtain a sample preparation solution.

[0048] Example 2

[0049] This embodiment provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the method comprises 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., hydrofluoric acid with a concentration of 50 wt%) was slowly added dropwise, the mass volume ratio of the high-purity titanium powder and the first acid was 0.5 g:3 mL, and after a first reaction was carried out at 40°C for 1.5 h, 6 mL of the second acid (i.e., hydrofluoric acid with a concentration of 25 wt%) was added at 20°C, the volume ratio of the first acid to the second acid was 4:6, and the second reaction was allowed to stand for 3 min. After the reaction was completed, 0.8 mL of a solvent (i.e., nitric acid) was added dropwise to the reaction product, and the volume ratio of the reaction product to the solvent was 10:0.8. The obtained solution was then transferred to a volumetric flask, and ultrapure water was added to make the volume up to 100 mL to obtain a sample preparation solution.

[0051] Example 3

[0052] This embodiment provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the method comprises 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., hydrofluoric acid with a concentration of 30 wt%) was slowly added dropwise, the mass volume ratio of the high-purity titanium powder and the first acid was 0.5 g:6 mL, and after a first reaction was carried out at 80°C for 0.5 h, 4 mL of the second acid (i.e., hydrofluoric acid with a concentration of 15 wt%) was added at 30°C, the volume ratio of the first acid to the second acid was 6:4, and the second reaction was allowed to stand for 8 min. After the reaction was completed, 1.2 mL of a solvent (i.e., nitric acid) was added dropwise to the reaction product, and the volume ratio of the reaction product to the solvent was 10:1.2. The obtained solution was then transferred to a volumetric flask, and ultrapure water was added to make the volume up to 100 mL to obtain a sample preparation solution.

[0054] Example 6

[0055] This embodiment provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the method comprises the following steps:

[0056] Place 0.5g of high-purity titanium powder in a polytetrafluoroethylene beaker, and then slowly add 5mL of the first acid (i.e., hydrofluoric acid with a concentration of 40wt%), the mass volume ratio of the high-purity titanium powder and the first acid is 0.5g:1mL, after a first reaction at 60°C for 1h, add 5mL of the second acid (i.e., hydrofluoric acid with a concentration of 20wt%) at 25°C, the volume ratio of the first acid to the second acid is 5:5, let stand for 5min for a second reaction, after the reaction is completed, add 1mL of a solvent (i.e., nitric acid) to the reaction product, the volume ratio of the reaction product to the solvent is 10:1, and then transfer the obtained solution to a volumetric flask, add ultrapure water to make the volume up to 100mL, and obtain a sample preparation solution.

[0057] Example 7

[0058] This embodiment provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the method comprises the following steps:

[0059] 0.5 g of high-purity titanium powder was placed in a polytetrafluoroethylene beaker, and then 5 mL of the first acid (i.e., hydrofluoric acid with a concentration of 40 wt%) was slowly added dropwise, the mass volume ratio of the high-purity titanium powder and the first acid was 0.5 g:10 mL, and after a first reaction was carried out at 60°C for 1 h, 5 mL of the second acid (i.e., hydrofluoric acid with a concentration of 20 wt%) was added at 25°C, the volume ratio of the first acid to the second acid was 5:5, and the second reaction was allowed to stand for 5 min. After the reaction was completed, 1 mL of a solvent (i.e., nitric acid) was added dropwise to the reaction product, and the volume ratio of the reaction product to the solvent was 10:1. The obtained solution was then transferred to a volumetric flask, and ultrapure water was added to make the volume up to 100 mL to obtain a sample preparation solution.

[0060] Example 8

[0061] This embodiment provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the method comprises the following steps:

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

[0063] Example 9

[0064] This embodiment provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the method comprises the following steps:

[0065] Place 0.5g of high-purity titanium powder in a polytetrafluoroethylene beaker, and then slowly add 5mL of the first acid (i.e., hydrofluoric acid with a concentration of 40wt%), the mass volume ratio of the high-purity titanium powder and the first acid is 0.5g:5mL, after a first reaction at 90°C for 1h, add 5mL of the second acid (i.e., hydrofluoric acid with a concentration of 20wt%) at 25°C, the volume ratio of the first acid to the second acid is 5:5, let stand for 5min for a second reaction, after the reaction is completed, add 1mL of a solvent (i.e., nitric acid) to the reaction product, the volume ratio of the reaction product to the solvent is 10:1, and then transfer the obtained solution to a volumetric flask, add ultrapure water to make the volume up to 100mL, and obtain a sample preparation solution.

[0066] Example 10

[0067] This embodiment provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the method comprises the following steps:

[0068] 0.5 g of high-purity titanium powder was placed in a polytetrafluoroethylene beaker, and then 5 mL of the first acid (i.e., hydrofluoric acid with a concentration of 40 wt%) was slowly added dropwise, the mass volume ratio of the high-purity titanium powder and the first acid was 0.5 g:5 mL. After a first reaction was carried out at 60°C for 1 h, 10 mL of the second acid (i.e., hydrofluoric acid with a concentration of 20 wt%) was added at 25°C, the volume ratio of the first acid to the second acid was 5:10, and the second reaction was allowed to stand for 5 min. After the reaction was completed, 1 mL of a 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, and the obtained solution was then transferred to a volumetric flask, and ultrapure water was added to make the volume up to 100 mL to obtain a sample preparation solution.

[0069] Embodiment 11

[0070] This embodiment provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the method comprises the following steps:

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

[0072] Example 12

[0073] This embodiment provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the method comprises the following steps:

[0074] Place 0.5 g of high-purity titanium powder in a polytetrafluoroethylene beaker, and then slowly add 5 mL of the first acid (i.e., hydrofluoric acid with a concentration of 40 wt%), the mass volume ratio of the high-purity titanium powder and the first acid is 0.5 g:5 mL. After a first reaction at 60°C for 1 h, add 5 mL of the second acid (i.e., hydrofluoric acid with a concentration of 20 wt%) at 15°C, the volume ratio of the first acid to the second acid is 5:5, and let stand for 5 min for a second reaction. After the reaction is completed, add 1 mL of a solvent (i.e., nitric acid) to the reaction product, the volume ratio of the reaction product to the solvent is 10:1, and then transfer the obtained solution to a volumetric flask, add ultrapure water to make the volume up to 100 mL, and obtain a sample preparation solution.

[0075] Embodiment 13

[0076] This embodiment provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the method comprises the following steps:

[0077] Place 0.5g of high-purity titanium powder in a polytetrafluoroethylene beaker, and then slowly add 5mL of the first acid (i.e., hydrofluoric acid with a concentration of 40wt%), the mass volume ratio of the high-purity titanium powder and the first acid is 0.5g:5mL, after a first reaction at 60°C for 1h, add 5mL of the second acid (i.e., hydrofluoric acid with a concentration of 20wt%) at 40°C, the volume ratio of the first acid to the second acid is 5:5, let stand for 5min for a second reaction, after the reaction is completed, add 1mL of a solvent (i.e., nitric acid) to the reaction product, the volume ratio of the reaction product to the solvent is 10:1, and then transfer the obtained solution to a volumetric flask, add ultrapure water to make the volume up to 100mL, and obtain a sample preparation solution.

[0078] Embodiment 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 rest of the sample preparation methods and parameters were the same as those in Example 1.

[0081] Embodiment 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 rest of the sample preparation methods and parameters were the same as those in Example 1.

[0084] Comparative Example 1

[0085] This comparative example provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the sample preparation method comprises the following steps:

[0086] Place 0.5 g of high-purity titanium powder in a polytetrafluoroethylene beaker, and then slowly add 5 mL of the first acid (i.e., hydrofluoric acid with a concentration of 40 wt%), the mass volume ratio of the high-purity titanium powder and the first acid is 0.5 g:5 mL, and carry out the first reaction at 60°C for 1 h. After the reaction, add 1 mL of solvent (i.e., nitric acid) to the reaction product, and 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 the volume up to 100 mL, and obtain a sample preparation solution.

[0087] Comparative Example 2

[0088] This comparative example provides a method for preparing a sample of high-purity titanium powder for particle size detection, and the sample preparation method comprises the following steps:

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

[0090] Performance Testing

[0091] The sample preparation solutions provided in the above embodiments and comparative examples are subjected to particle size detection to calculate the standard deviation, and the specific steps include:

[0092] (a) 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, proceed to the subsequent steps.

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

[0094] (c) The particle count of the high purity titanium powder was performed three times to calculate the standard deviation.

[0095] The results are shown in Table 1.

[0096] Table 1

[0097]

[0098]

[0099] analyze:

[0100] As can be seen from the above table, the sample preparation method provided by the present invention can not only ensure that no pollution is introduced during the sample preparation process, so that the test results truly reflect the particle size distribution of titanium powder and improve the accuracy of particle size detection, but also the sample preparation method has high stability and high efficiency, and can complete the sample preparation in a relatively short time, thereby improving the detection efficiency. In addition, the sample preparation method has strong operability and high safety, reduces the difficulty and cost of sample preparation, and is easy to promote and apply.

[0101] The applicant declares that the present invention illustrates the process method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned process steps, that is, it does not mean that the present invention must rely on the above-mentioned process steps to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials selected by 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 method for preparing a sample of high-purity titanium powder for particle size detection, characterized in that: The sample preparation method comprises the following steps: (1) mixing high-purity titanium powder and a first acid to carry out a first reaction, and adding a second acid after the reaction to carry out a second reaction to obtain a reaction product; (2) The reaction product and a solvent are mixed, and then the volume is fixed to obtain a sample preparation solution.

2. The sample preparation method according to claim 1, characterized in that: The purity of the high-purity titanium powder in step (1) is ≥99.5%; Preferably, the mass volume ratio of the high purity titanium powder and the first acid in step (1) is 0.5 g: (2-8) mL; Preferably, in step (1), the first acid comprises hydrofluoric acid; Preferably, the concentration of the first acid in step (1) is 30-50 wt%.

3. The sample preparation method according to claim 1 or 2, characterized in that: Step (1) The temperature of the first reaction is 40-80°C; Preferably, the time of the first reaction in step (1) is 0.5-1.5 h.

4. The sample preparation method according to any one of claims 1 to 3, characterized in that: Step (1) the second acid comprises hydrofluoric acid; Preferably, the concentration of the second acid in step (1) is 15-25 wt %; Preferably, in step (1), the volume ratio of the first acid to the second acid is (4-6):(6-4).

5. The sample preparation method according to any one of claims 1 to 4, characterized in that: The temperature of the second reaction in step (1) is 20-30°C; Preferably, the time of the second reaction in step (2) is 3-8 min.

6. The sample preparation method according to any one of claims 1 to 5, characterized in that: The dissolving agent in step (2) comprises nitric acid; Preferably, the volume ratio of the reaction product to the solvent in step (2) is 10:(0.8-1.2).

7. The sample preparation method according to any one of claims 1 to 6, characterized in that: The sample preparation method comprises the following steps: Place high-purity titanium powder with a purity of ≥99.5% in a beaker, and then slowly add the first acid dropwise, the mass volume ratio of the high-purity titanium powder and the first acid is 0.5g:(2-8)mL, carry out the first reaction at 40-80°C for 0.5-1.5h, then add the second acid at 20-30°C, the volume ratio of the first acid to the second acid is (4-6):(6-4), and carry out the second reaction for 3-8min. After the reaction, add the solvent dropwise to the reaction product, the volume ratio of the reaction product to the solvent is 10:(0.8-1.2), and then transfer the obtained solution to a volumetric flask, add water to make up the volume, and obtain a sample preparation solution.

8. Use of a sample preparation solution obtained by the sample preparation method according to any one of claims 1 to 7 in particle size detection.

9. The use according to claim 8, characterized in that: The steps of applying the sample preparation solution in particle size detection include: The liquid particle counter is pre-treated, and then the sampling tube of the liquid particle counter is inserted into the sample preparation solution for detection. The detection is performed multiple times and the average value is taken to obtain the detection result.

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