Granularity detection method for copper alloy

Abstract

The invention relates to a granularity detection method of a copper alloy. The detection method comprises the following steps: (1) processing a copper alloy target material to be detected into a copper wire; (2) the copper wire obtained in the step (1) is subjected to acid pickling, water washing and alcohol washing in sequence, and an alcohol washing sample is obtained; (3) dissolving the alcohol-washed sample obtained in the step (2) by using a nitric acid solution and ultrapure water to obtain a sample to be detected; and (4) carrying out granularity detection on the to-be-detected sample obtained in the step (3) by using a KS-42C liquid particle counter. By using KS-42C, the number of particles with the particle size ranging from 0.5 mu m to 20 mu m can be detected, the precision is higher, detection can be carried out without diluting a to-be-detected sample, the influence of a background is weakened, and the detection result is more accurate.

Description

Technical Field

[0001] The invention belongs to the field of detection technology and relates to a particle size detection method, in particular to a copper alloy particle size detection method. Background Art

[0002] With the widespread application of chips, the demand for chips in the market has increased, and the demand for the four mainstream thin-film metal materials in the industry, namely aluminum, titanium, tantalum and copper, has also increased to a certain extent; high-purity copper and copper alloy targets are the main products in the sputtering target market. It is of great significance to achieve particle size distribution and size detection of high-purity copper alloys with a purity of ≥99.99wt%.

[0003] Liquid Particle Counter (LPC) is a device for detecting the number of suspended particles and particle size distribution in liquids. It can be used for quality control in the field of particle technology. It has a wide detection range and can detect samples with particle sizes of 1.3-20μm through interchangeable sensors. At the same time, LPC is simple to operate and easy to sample. It is widely used in medical-grade scientific research tests and the detection of insoluble matter in metals.

[0004] When detecting insoluble matter, the commonly used LPC is Beckman HIAC 9703+ liquid particle counter, but HIAC9703+ is widely used in the biomedical field and less used in the field of semiconductor metal detection; in addition, its detection range is 1.3-20μm, and the detection accuracy is low, which cannot meet the particle verification of copper alloy raw materials; moreover, when HIAC 9703+ is tested, the sample needs to be diluted to 1000 times, which causes high background impact and poor data reproducibility; in addition, the sampling needle of HIAC 9703+ is made of 316 stainless steel, which is not resistant to strong acids and alkalis, and is prone to rust and blockage after long-term use, affecting the test results; the analytical pure nitric acid used in the test process has a high impurity content and a large particle content, which has a greater impact on the test results; and the ordinary pure water used in the test process has a high resistivity, which also affects the test results.

[0005] Therefore, it is necessary to provide a method for detecting the particle size of copper alloy to overcome the defects when using HIAC 9703+ liquid particle counter. Summary of the invention

[0006] The object of the present invention is to provide a method for detecting the particle size of a copper alloy. The method is suitable for detecting the liquid particle size of a copper alloy with a purity of 99.99wt% or more, has high detection accuracy, and can effectively reduce the influence of background.

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

[0008] The present invention provides a method for detecting the particle size of a copper alloy, the method comprising the following steps:

[0009] (1) Processing the copper alloy target to be tested into copper wire;

[0010] (2) sequentially acid-washing, water-washing and alcohol-washing the copper wire obtained in step (1) to obtain an alcohol-washed sample;

[0011] (3) using nitric acid solution and ultrapure water to dissolve the alcohol-washed sample obtained in step (2) to obtain a sample to be tested;

[0012] (4) Use a KS-42C liquid particle counter to measure the particle size of the sample obtained in step (3).

[0013] The liquid particle counter is a device for detecting the number of suspended particles in a liquid and the distribution of particle sizes. The KS-42C liquid particle counter can detect the number of particles within 0.5-20μm. It uses light scattering. When a light beam is suspended in a liquid, part of the light is absorbed, while the other part is scattered. By measuring the change of the scattered light intensity with the scattering angle, the size and distribution of the particles can be determined. The present invention can detect the number of particles within the range of 0.5-20μm in particle size by using KS-42C, with higher accuracy, and can detect without diluting the sample to be tested, which reduces the influence of the background and makes the detection result more accurate.

[0014] Preferably, the length of the copper wire in step (1) is 0.8-1.2 cm.

[0015] Preferably, the pickling in step (2) uses 30-50wt% nitric acid.

[0016] Preferably, the pickling time in step (2) is 2.5-3.5 min.

[0017] Preferably, the number of times of washing with water in step (2) is 3 or more times.

[0018] Preferably, the alcohol washing in step (2) is ultrasonic cleaning using anhydrous ethanol.

[0019] Preferably, the alcohol washing time in step (2) is 25-35s.

[0020] Preferably, the alcohol washing in step (2) is followed by drying to remove residual anhydrous ethanol.

[0021] Preferably, the concentration of the nitric acid solution in step (3) is 45-55wt%.

[0022] Preferably, the volume ratio of the nitric acid solution to ultrapure water in step (3) is 1:(1.4-1.6).

[0023] Preferably, the volume mass ratio of the nitric acid solution to the alcohol-washed sample in step (3) is (9-11) mL:1 g.

[0024] Preferably, the particle size detection in step (4) includes:

[0025] First, use ultrapure water for testing. When the test is within the standard range, use a liquid particle counter sampling tube for testing. Sampling is performed at least 3 times, and the average value is the test result.

[0026] As a preferred technical solution of the particle size detection method provided by the present invention, the particle size detection method comprises the following steps:

[0027] (1) Processing the copper alloy target to be tested into a copper wire with a length of 0.8-1.2 cm;

[0028] (2) sequentially acid-washing, water-washing and alcohol-washing the copper wire obtained in step (1), and drying to remove residual anhydrous ethanol to obtain an alcohol-washed sample;

[0029] The pickling is carried out using 30-50wt% nitric acid for 2.5-3.5min;

[0030] The number of times of washing is more than 3 times;

[0031] The alcohol washing is ultrasonic cleaning with anhydrous ethanol for 25-35s;

[0032] (3) using a nitric acid solution having a concentration of 45-55 wt % and ultrapure water to dissolve the alcohol-washed sample obtained in step (2) to obtain a sample to be tested;

[0033] The volume ratio of the nitric acid solution to ultrapure water is 1:(1.4-1.6);

[0034] The volume mass ratio of the nitric acid solution to the alcohol-washed sample is (9-11) mL:1 g

[0035] (4) Use a KS-42C liquid particle counter to test the particle size of the sample obtained in step (3): first use ultrapure water for testing. When the test is within the standard range, use a liquid particle counter sampling tube for testing. Sampling is performed at least 3 times, and the average value obtained is the test result.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] The liquid particle counter is a device for detecting the number of suspended particles in a liquid and the distribution of particle sizes. The KS-42C liquid particle counter can detect the number of particles within 0.5-20μm. It uses light scattering. When a light beam is suspended in a liquid, part of the light is absorbed, while the other part is scattered. By measuring the change of the scattered light intensity with the scattering angle, the size and distribution of the particles can be determined. The present invention can detect the number of particles within the range of 0.5-20μm in particle size by using KS-42C, with higher accuracy, and can detect without diluting the sample to be tested, which reduces the influence of the background and makes the detection result more accurate. DETAILED DESCRIPTION

[0038] 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.

[0039] A certain embodiment of the present invention provides a method for detecting the particle size of a copper alloy, the method comprising the following steps:

[0040] (1) Processing the copper alloy target to be tested into copper wire;

[0041] (2) sequentially acid-washing, water-washing and alcohol-washing the copper wire obtained in step (1) to obtain an alcohol-washed sample;

[0042] (3) using nitric acid solution and ultrapure water to dissolve the alcohol-washed sample obtained in step (2) to obtain a sample to be tested;

[0043] (4) Use a KS-42C liquid particle counter to measure the particle size of the sample obtained in step (3).

[0044] The liquid particle counter is a device for detecting the number of suspended particles in a liquid and the distribution of particle sizes. The KS-42C liquid particle counter can detect the number of particles within 0.5-20μm. It uses light scattering. When a light beam is suspended in a liquid, part of the light is absorbed, while the other part is scattered. By measuring the change of the scattered light intensity with the scattering angle, the size and distribution of the particles can be determined. The present invention can detect the number of particles within the range of 0.5-20μm in particle size by using KS-42C, with higher accuracy, and can detect without diluting the sample to be tested, which reduces the influence of the background and makes the detection result more accurate.

[0045] In some embodiments, the length of the copper wire in step (1) is 0.8-1.2 cm, for example, 0.8 cm, 0.9 cm, 1 cm, 1.1 cm or 1.2 cm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0046] In certain embodiments, the pickling in step (2) uses 30-50wt% nitric acid, for example, 30wt%, 35wt%, 40wt%, 45wt% or 50wt%, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0047] In some embodiments, the pickling time in step (2) is 2.5-3.5 min, for example, 2.5 min, 2.8 min, 3 min, 3.2 min or 3.5 min, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0048] In some embodiments, the number of water washings in step (2) is more than 3 times, for example, 3 times, 4 times, 5 times or 6 times, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0049] The present invention removes the residual nitric acid by water washing in step (2). The more times of water washing, the better the effect of removing the residual nitric acid. However, too many times of water washing will increase the sample preparation time of the particle size detection method, which is not conducive to improving the detection efficiency.

[0050] In certain embodiments, the alcohol washing in step (2) is ultrasonic cleaning using anhydrous ethanol.

[0051] In some embodiments, the alcohol washing time in step (2) is 25-35 s, for example, 25 s, 28 s, 30 s, 32 s or 35 s, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0052] In some embodiments, the alcohol washing in step (2) is followed by drying to remove residual anhydrous ethanol.

[0053] In some embodiments, the concentration of the nitric acid solution in step (3) is 45-55wt%, for example, 45wt%, 48wt%, 50wt%, 52wt% or 54wt%, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0054] In certain embodiments, the volume ratio of the nitric acid solution to ultrapure water in step (3) is 1:(1.4-1.6), for example, it can be 1:1.4, 1:1.5 or 1:1.6, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0055] In certain embodiments, the volume mass ratio of the nitric acid solution to the alcohol-washed sample in step (3) is (9-11) mL:1 g, for example, 9 mL:1 g, 10 mL:1 g or 11 mL:1 g, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0056] In some embodiments, the particle size detection in step (4) includes:

[0057] First, use ultrapure water for testing. When the test is within the standard range, use a liquid particle counter sampling tube for testing. Sampling is performed at least 3 times, and the average value is the test result.

[0058] A particle size detection method provided by an embodiment of the present invention comprises the following steps:

[0059] (1) Processing the copper alloy target to be tested into a copper wire with a length of 0.8-1.2 cm;

[0060] (2) sequentially acid-washing, water-washing and alcohol-washing the copper wire obtained in step (1), and drying to remove residual anhydrous ethanol to obtain an alcohol-washed sample;

[0061] The pickling is carried out using 30-50wt% nitric acid for 2.5-3.5min;

[0062] The number of times of washing is more than 3 times;

[0063] The alcohol washing is ultrasonic cleaning with anhydrous ethanol for 25-35s;

[0064] (3) using a nitric acid solution having a concentration of 45-55 wt % and ultrapure water to dissolve the alcohol-washed sample obtained in step (2) to obtain a sample to be tested;

[0065] The volume ratio of the nitric acid solution to ultrapure water is 1:(1.4-1.6);

[0066] The volume mass ratio of the nitric acid solution to the alcohol-washed sample is (9-11) mL:1 g

[0067] (4) Use a KS-42C liquid particle counter to test the particle size of the sample obtained in step (3): first use ultrapure water for testing. When the test is within the standard range, use a liquid particle counter sampling tube for testing. Sampling is performed at least 3 times, and the average value obtained is the test result.

[0068] Example 1

[0069] This embodiment provides a method for detecting the particle size of a copper alloy, and the particle size detection method comprises the following steps:

[0070] (1) Processing the copper alloy target to be tested into a copper wire with a length of 1 cm;

[0071] (2) sequentially acid-washing, water-washing and alcohol-washing the copper wire obtained in step (1), and drying to remove residual anhydrous ethanol to obtain an alcohol-washed sample;

[0072] The pickling is carried out using 40wt% nitric acid for 3min;

[0073] The number of times of washing is 3 times;

[0074] The alcohol washing is ultrasonic cleaning with anhydrous ethanol for 30 seconds;

[0075] (3) taking 4 g of the alcohol-washed sample, dissolving the alcohol-washed sample obtained in step (2) in a 50 wt % nitric acid solution, and then adding ultrapure water to obtain a sample to be tested;

[0076] The volume ratio of the nitric acid solution to ultrapure water is 1:1.5;

[0077] The volume mass ratio of the nitric acid solution to the alcohol-washed sample is 10 mL:1 g

[0078] (4) Use a KS-42C liquid particle counter to test the particle size of the sample obtained in step (3): First, use ultrapure water for testing. When the test is within the standard range, use a liquid particle counter sampling tube for testing. Take samples three times, each time taking 10 mL, and the average value is the test result.

[0079] This embodiment uses KS-42C to detect the number of particles in the range of 0.5-20 μm in diameter with higher accuracy, and can perform detection without diluting the sample to be tested, thereby reducing the impact of the background and making the detection result more accurate.

[0080] Example 2

[0081] This embodiment provides a method for detecting the particle size of a copper alloy, and the particle size detection method comprises the following steps:

[0082] (1) Processing the copper alloy target to be tested into a copper wire with a length of 0.8 cm;

[0083] (2) sequentially acid-washing, water-washing and alcohol-washing the copper wire obtained in step (1), and drying to remove residual anhydrous ethanol to obtain an alcohol-washed sample;

[0084] The pickling is carried out using 30wt% nitric acid for 3.5min;

[0085] The number of times of washing is 3 times;

[0086] The alcohol washing is ultrasonic cleaning with anhydrous ethanol for 25 seconds;

[0087] (3) taking 4 g of the alcohol-washed sample, dissolving the alcohol-washed sample obtained in step (2) in a 45 wt % nitric acid solution, and then adding ultrapure water to obtain a sample to be tested;

[0088] The volume ratio of the nitric acid solution to ultrapure water is 1:1.4;

[0089] The volume mass ratio of the nitric acid solution to the alcohol-washed sample is 9 mL:1 g

[0090] (4) Use a KS-42C liquid particle counter to test the particle size of the sample obtained in step (3): First, use ultrapure water for testing. When the test is within the standard range, use a liquid particle counter sampling tube for testing. Take samples three times, each time taking 10 mL, and the average value is the test result.

[0091] This embodiment uses KS-42C to detect the number of particles in the range of 0.5-20 μm in diameter with higher accuracy, and can perform detection without diluting the sample to be tested, thereby reducing the impact of the background and making the detection result more accurate.

[0092] Example 3

[0093] This embodiment provides a method for detecting the particle size of a copper alloy, and the particle size detection method comprises the following steps:

[0094] (1) Processing the copper alloy target to be tested into a copper wire with a length of 1.2 cm;

[0095] (2) sequentially acid-washing, water-washing and alcohol-washing the copper wire obtained in step (1), and drying to remove residual anhydrous ethanol to obtain an alcohol-washed sample;

[0096] The pickling is carried out using 50wt% nitric acid for 2.5min;

[0097] The number of times of washing is 3 times;

[0098] The alcohol washing is ultrasonic cleaning with anhydrous ethanol for 35 seconds;

[0099] (3) taking 4 g of the alcohol-washed sample, dissolving the alcohol-washed sample obtained in step (2) in a 45 wt % nitric acid solution, and then adding ultrapure water to obtain a sample to be tested;

[0100] The volume ratio of the nitric acid solution to ultrapure water is 1:1.6;

[0101] The volume mass ratio of the nitric acid solution to the alcohol-washed sample is 11 mL:1 g

[0102] (4) Use a KS-42C liquid particle counter to test the particle size of the sample obtained in step (3): First, use ultrapure water for testing. When the test is within the standard range, use a liquid particle counter sampling tube for testing. Take samples three times, each time taking 10 mL, and the average value is the test result.

[0103] This embodiment uses KS-42C to detect the number of particles in the range of 0.5-20 μm in diameter with higher accuracy, and can perform detection without diluting the sample to be tested, thereby reducing the impact of the background and making the detection result more accurate.

[0104] In summary, a liquid particle counter is a device for detecting the number of suspended particles in a liquid and the distribution of particle sizes. The KS-42C liquid particle counter can detect the number of particles within 0.5-20 μm. It uses light scattering. When a light beam is suspended in a liquid, part of the light is absorbed, while the other part of the light is scattered. By measuring the change of the scattered light intensity with the scattering angle, the size and distribution of the particles can be determined. The present invention can detect the number of particles within the range of 0.5-20 μm in particle size by using KS-42C, with higher accuracy, and can detect without diluting the sample to be tested, thereby reducing the influence of the background and making the detection result more accurate.

[0105] The above description is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention are within the protection scope and disclosure scope of the present invention.

Claims

1. A method for detecting the particle size of a copper alloy, characterized in that: The particle size detection method comprises the following steps: (1) Processing the copper alloy target to be tested into copper wire; (2) sequentially acid-washing, water-washing and alcohol-washing the copper wire obtained in step (1) to obtain an alcohol-washed sample; (3) using nitric acid solution and ultrapure water to dissolve the alcohol-washed sample obtained in step (2) to obtain a sample to be tested; (4) Use a KS-42C liquid particle counter to measure the particle size of the sample obtained in step (3).

2. The particle size detection method according to claim 1, characterized in that: The length of the copper wire in step (1) is 0.8-1.2 cm.

3. The particle size detection method according to claim 1 or 2, characterized in that: The pickling in step (2) uses 30-50wt% nitric acid; Preferably, the pickling time in step (2) is 2.5-3.5 min.

4. The particle size detection method according to any one of claims 1 to 3, characterized in that: The number of times of washing with water in step (2) is more than 3 times.

5. The particle size detection method according to any one of claims 1 to 4, characterized in that: The alcohol washing in step (2) is ultrasonic cleaning using anhydrous ethanol; Preferably, the alcohol washing time in step (2) is 25-35s.

6. The particle size detection method according to claim 5, characterized in that: The alcohol washing in step (2) is followed by drying to remove residual anhydrous ethanol.

7. The particle size detection method according to any one of claims 1 to 6, characterized in that: The concentration of the nitric acid solution in step (3) is 45-55wt%.

8. The particle size detection method according to claim 7, characterized in that: The volume ratio of the nitric acid solution to ultrapure water in step (3) is 1:(1.4-1.6); Preferably, the volume mass ratio of the nitric acid solution to the alcohol-washed sample in step (3) is (9-11) mL:1 g.

9. The particle size detection method according to any one of claims 1 to 8, characterized in that: The particle size detection in step (4) includes: First, use ultrapure water for testing. When the test is within the standard range, use a liquid particle counter sampling tube for testing. Sampling is performed at least 3 times, and the average value is the test result.

10. The particle size detection method according to any one of claims 1 to 9, characterized in that: The particle size detection method comprises the following steps: (1) Processing the copper alloy target to be tested into a copper wire with a length of 0.8-1.2 cm; (2) sequentially acid-washing, water-washing and alcohol-washing the copper wire obtained in step (1), and drying to remove residual anhydrous ethanol to obtain an alcohol-washed sample; The pickling is carried out using 30-50wt% nitric acid for 2.5-3.5min; The number of times of washing is more than 3 times; The alcohol washing is ultrasonic cleaning with anhydrous ethanol for 25-35s; (3) using a nitric acid solution having a concentration of 45-55 wt % and ultrapure water to dissolve the alcohol-washed sample obtained in step (2) to obtain a sample to be tested; The volume ratio of the nitric acid solution to ultrapure water is 1:(1.4-1.6); The volume mass ratio of the nitric acid solution to the alcohol-washed sample is (9-11) mL:1 g (4) Use a KS-42C liquid particle counter to perform particle size detection on the sample obtained in step (3): First, use ultrapure water for detection. When the detection is within the standard range, use a liquid particle counter sampling tube for detection. Sampling is performed at least 3 times, and the average value obtained is the detection result.