CN115753567A - Analysis method for counting particles of copper or copper alloy - Google Patents
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Abstract
The invention relates to the technical field of particle calculation, in particular to an analysis method for counting particles of copper or copper alloy. The solution to be measured is neutral, and the possibility of continuous reaction generation or reduction of particles in acid liquor can not occur, so that the stability of the particles in the solution is ensured, meanwhile, because the inclusion size of particles in the ultra-high pure copper is generally less than 2 mu m, the possibility of agglomeration exists in the solution due to the fact that the particle size of more particles is in the submicron order, the surfactant is added, the fine particles can be effectively dispersed, and the granularity of the copper or copper alloy material in the solution to be measured can be accurately analyzed and calculated.
Description
Technical Field
The invention relates to the technical field of particle calculation, in particular to an analysis method for counting particles of copper or copper alloy.
Background
Copper or copper alloy is a key interconnection line material of an integrated circuit below 90nm, and is mainly prepared by sputtering a copper or copper alloy target material, and the deposition process and the performance of the target material are influenced by the purity and inclusion defects of the target material in the process of sputtering the target material to form a film. The lower impurity content of copper or copper alloy means better conductivity and better signal transmission performance. The higher the purity of the copper or copper alloy target material is, the better the electrical property of the film is, and along with the reduction of the line width of an integrated circuit, the purity requirement of the copper or copper alloy target material is higher and higher, and the requirement reaches 6N (not less than 99.9999 percent) and even 7N (not less than 99.99999 percent), although the precision of detecting the content of metal impurity elements by adopting a Glow Discharge Mass Spectrometry (GDMS) is very high, particles (particles) caused by some non-metal impurities such as alumina, carbon and carbide in the sputtering process may exist in the actual preparation process of the copper or copper alloy, so that the coating film fails. These micro-inclusions are difficult to analyze by GDMS and LECO, etc., and some non-metallic inclusions such as alumina, carbon and carbide may be present in the actual copper or copper alloy target material to cause Particle during sputtering, resulting in coating failure. For non-metallic inclusions in copper or copper alloy target materials, establishing and detecting insoluble particles of copper or copper alloy and establishing an LPC detection method by utilizing a Liquid Particle Counter (LPC) is necessary.
Liquid particle counters are mainly used to measure the amount of insoluble particles in a liquid, and there are two methods, one is a photoresist method and the other is a light scattering method.
The principle of the photo-resist method: the liquid to be measured flows through a flow cell with a small cross section, optical glass is arranged on two sides of the flow cell, and light beams of the laser are collimated through a lens group, pass through the flow cell and are received by a photoelectric detector. If there is particle matter in the liquid, the particle will block the laser through the sensing area of the flow cell, the optical signal received by the photoelectric detector is reduced, and a negative pulse electrical signal is generated, the amplitude of the pulse signal corresponds to the size of the particle, and the number of the pulse signal corresponds to the number of the particles.
Principle of light scattering method: the liquid to be measured flows through the flow cell, optical glass is arranged on two sides of the flow cell, light beams of the laser are collimated through the lens group, and the light beams penetrate through the flow cell and irradiate on the light trap. If no particles exist in the liquid to be detected, the photoelectric detector cannot receive the optical signal, and if particles exist in the liquid, the particles pass through the flow cell and scatter with the laser beam. Scattered light under a certain angle (or a plurality of angles) is collected by a lens and converged on a photoelectric detector to generate a positive electric signal pulse, and the amplitude of the pulse signal is in direct proportion to the intensity of the scattered light. According to the amplitude and number of the signals, the counting detection of the tiny particles in the liquid can be carried out. The liquid particle counter has the following food and medicine qualities: infusion solution, medicinal water, purified water, etc. Detecting the quality of oil products: hydraulic oil, lubricating oil, transformer oil, turbine oil, gear oil, engine oil, aviation kerosene, and the like. Industry and research: evaluating the performance of the filter material, and testing the counting and particle size distribution of various powder materials. And the application range is wide.
CN 102165093B "sputtering target of high purity copper and high purity copper alloy, method for producing the sputtering target, and sputtering film of high purity copper or high purity copper alloy" patent, it is mentioned that non-metal inclusions in copper are measured by using "automatic particle counter of liquid light scattering type", but it does not relate to a specific method for detecting particles of high purity copper material.
EP 2330231B1, PROCESS FOR MANUFACTURING A HIGH-PURITY COPPER-OR A HIGH-PURITY COPPER ALLOY SPUTTERING TARGET the above mentioned carbon-based inclusions of non-metallic inclusions OR carbon OR carbides are measured with a "liquid light-scattering auto-particle counter" (the standard FOR examination can be referred to JIS B9925-2010 liquid light-scattering auto-particle counter). The measurement method is based on classifying the particle size in the liquid and measuring the particle concentration and the particle count. The above-mentioned measuring apparatus is also referred to as a "liquid particle counter", based on JIS B9925 (the measuring apparatus is hereinafter referred to as a "liquid particle counter"). But does not relate to a specific detection method of particles of copper or copper alloy materials.
Disclosure of Invention
The analysis method comprises the steps of mixing nitric acid and pure water according to a certain proportion, reacting with a copper or copper alloy material in a reaction container at normal temperature, dissolving the copper or copper alloy material, neutralizing a copper nitrate solution by using an alkaline reagent, adding a surfactant, performing constant volume shaking uniformly to obtain a solution to be detected, and analyzing and calculating the granularity of the copper or copper alloy material in the solution to be detected. The method specifically comprises the following steps:
an analytical method for particle counting of copper or copper alloys comprising the steps of:
(1) Sampling copper or copper alloy to obtain a copper or copper alloy sample, and then pretreating the copper or copper alloy sample;
(2) Preparing an etching solution by mixing nitric acid and pure water according to a volume ratio of (0.6-1.2) to 1, wherein the volume ratio of nitric acid to pure water can be 0.6;
(3) Dissolving a copper or copper alloy sample in a corrosive liquid at the temperature of 20-26 ℃ to obtain a copper nitrate solution; the proportion of the copper or copper alloy sample to the corrosive liquid is (0.08-0.12) g:1mL; specifically, the ratio of the copper or copper alloy sample to the corrosive liquid may be 0.08g; the dissolution temperature may be 23 deg.C, 23.5 deg.C, 24 deg.C, 24.5 deg.C, 25 deg.C, etc.;
(4) Adjusting the pH of the copper nitrate solution to =7 by using an alkaline reagent, then adding a surfactant into the solution, and performing constant volume shaking to obtain a solution to be detected;
(5) And taking the solution to be detected, sampling, detecting on a computer and processing data in sequence, and detecting the number of particles in the solution to be detected so as to obtain the granularity of the copper or the copper alloy.
The analysis method for counting the particles of the copper or the copper alloy can be applied to counting the insoluble particles in the copper or the copper alloy. The solution prepared by the method is a neutral solution, and the surfactant is added, so that the stability of the state of particles in the solution is improved, the data are more stable, and the acid and alkali resistance of equipment is more friendly. In the invention, the solution to be tested is sampled, tested on a computer and processed with data in sequence, namely 10mL of the solution to be tested is taken for on-computer test, repeated for three times or more in parallel, and the average value is taken; mixing nitric acid and pure water according to the same volume ratio to form a blank solution with the same ratio as the sample solution, taking 10ml of the blank solution, detecting on a machine, repeating for three times or more in parallel, taking an average value, and subtracting a detection value obtained by the blank sample from a detection value obtained by the solution to be detected to obtain the actual particle content of the sample.
Preferably, the purity of the copper or copper alloy in the step (1) is more than or equal to 99.9999wt%, for example, 99.9999wt%, 99.99992wt%, 99.99994wt%, 99.9999996 wt%, 99.99998wt%, 99.99999wt%, etc. can be obtained.
Preferably, the copper or copper alloy sample in the step (1) is a columnar sample. The method comprises the steps of taking copper or copper alloy into a columnar sample, dissolving the sample in acid liquor through the steps of acid washing, corrosion and the like, neutralizing with an alkaline reagent, adding a surfactant to form mixed sample liquid, detecting the granularity of the sample liquid, and calculating to obtain a final result. Copper or copper alloy is a columnar sample, and compared with a scrap-shaped sample, the columnar sample has smaller area, surface pollution is easy to remove, the reaction speed is easy to control, and the detection precision is improved.
Preferably, the specification of the columnar sample is phi 2-5mm x 5mm.
Preferably, the pretreatment method in step (1) is: and washing the copper or copper alloy sample by using dilute nitric acid for 3-5min.
Preferably, the concentration of the nitric acid in the step (2) is 65 to 68wt%.
Preferably, the dissolving time in the step (3) is 1-2.5h, such as 1h, 1.2h, 1.4h, 1.8h, 2.0h, 2.2h, 2.5h and the like.
Preferably, the alkaline reagent in step (4) is electronic grade triethanolamine or ammonium hydroxide.
Preferably, the surfactant in step (4) is one or more of polysorbate 20, polysorbate 80, or Triton X-100.
Preferably, the mass concentration of the surfactant in the step (4) is 0.05-1% (e.g., 0.05%, 0.08%, 0.1%, 0.3%, 0.5%, 0.8%, 1%, etc.); the ratio of surfactant to copper nitrate solution was (0.8-1.2) mL:100mL, e.g., 0.8: 100. 1.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) Preparing a columnar sample with the size specification of phi 2-5mm x 5mm, which is copper or copper alloy with the purity of more than or equal to 99.9999wt%, washing the prepared copper or copper alloy for 3-5min by using dilute nitric acid with the volume ratio of the nitric acid to the pure water of 1:1, wherein the concentration of the nitric acid is 65-68wt%, and obtaining the pretreated copper or copper alloy;
(2) Mixing nitric acid and pure water according to the volume ratio of (0.8-1) to 1 to obtain a corrosion solution, mixing the copper or copper alloy pretreated in the step (1) and the corrosion solution according to the ratio of (0.08-0.12) g:1mL, dissolving a sample in a reaction container at normal temperature for 1-2.5h, neutralizing the copper nitrate solution with an alkaline reagent until the pH value is =7 after complete dissolution, adding a surfactant, and performing constant volume shaking to obtain a solution to be measured;
(3) And (3) sequentially sampling, carrying out on-machine detection and carrying out data processing on the solution to be detected in the step (2) to obtain the granularity of the copper or the copper alloy.
The invention has the beneficial effects that:
(1) The invention provides an analysis method for counting particles of copper or copper alloy, which comprises the steps of mixing nitric acid and pure water according to a certain proportion, reacting with a copper or copper alloy material at normal temperature, dissolving the copper or copper alloy material in the nitric acid solution, neutralizing the copper nitrate solution by using an alkaline reagent, adding a surfactant, and carrying out constant volume shaking to obtain a solution to be measured. The solution to be measured is neutral, and the possibility of continuous reaction generation or reduction of particles in acid liquor can not occur, so that the stability of the particles in the solution is ensured, meanwhile, because the inclusion size of particles in ultra-high pure copper is usually less than 2 mu m, the size of more particles is in submicron order, the possibility of agglomeration exists in the solution, and the surfactant is added, so that the fine particles can be effectively dispersed, and further, the granularity of the copper or copper alloy material in the solution to be measured can be accurately analyzed and calculated.
(2) According to the analysis method for counting the particles of the copper or the copper alloy, the RSD of the unneutralized sample preparation solution and the RSD of the original detection value are 4.9 after the unneutralized sample preparation solution is placed for 20min, the alkaline reagent is added for neutralizing the sample preparation, the surface active agent is added, and the RSD of the unneutralized sample preparation solution and the RSD of the original detection value are 1.2 after the unneutralized sample preparation solution is placed for 20min, so that the stability of the state of the particles in the solution is improved, the data are more stable, and the selection of the acid and alkali resistance of equipment is more friendly.
(3) The analysis method for counting the particles of the copper or the copper alloy is simple and easy to operate.
Detailed Description
The present invention will be described in detail with reference to the following embodiments. The embodiments shown below do not limit the inventive content described in the claims. The entire contents of the configurations shown in the following embodiments are not limited to those required as solutions of the inventions described in the claims.
Example 1
The present embodiment provides an analysis method for counting particles of copper or copper alloy, the analysis method comprising the steps of:
(1) Preparing a copper alloy with the purity of more than or equal to 99.9999wt% into a columnar sample with the size specification of phi 5 x 5mm, and washing the copper or the copper alloy after sample preparation for 5min by using dilute nitric acid with the volume ratio of the nitric acid to the pure water of 1:1, wherein the concentration of the nitric acid is 66.5wt%, so as to obtain the pretreated copper alloy;
(2) Mixing nitric acid and pure water according to the volume ratio of 0.8 to 1 to obtain an etching solution, mixing the pretreated copper or copper alloy obtained in the step (1) with the etching solution according to the volume ratio of 0.08g to 1mL, dissolving a sample in a reaction vessel at the normal temperature of 25 ℃ for 2.5h, neutralizing the copper nitrate solution with ammonium hydroxide to pH =7 after complete dissolution, and mixing the copper nitrate solution with the pure water according to the volume ratio of 1.0 mL: adding 1% Triton X-100 solution into 100mL of copper nitrate solution, and shaking up to constant volume to obtain a solution to be detected;
(3) And (3) sequentially sampling, detecting on a computer and processing data of the solution to be detected in the step (2) to obtain the granularity of the copper alloy.
The machine-up detection process in this example used a Bettersize C400 optical particle counter.
Example 2
The present embodiment provides an analysis method for counting particles of copper or copper alloy, the analysis method comprising the steps of:
(1) Preparing a copper alloy with the purity of more than or equal to 99.9999wt% into a columnar sample with the size specification of phi 4 x 5mm, and washing the copper or the copper alloy after sample preparation for 4min by using dilute nitric acid with the volume ratio of the nitric acid to the pure water of 1:1, wherein the concentration of the nitric acid is 66.5wt%, so as to obtain the pretreated copper or the copper alloy;
(2) Mixing nitric acid and pure water according to the volume ratio of 1:1 to obtain an etching solution, mixing the copper alloy pretreated in the step (1) with the etching solution according to the ratio of 0.10g to 1mL, dissolving the sample for 1.0h at normal temperature in a reaction container, neutralizing the copper nitrate solution with triethanolamine until the pH is =7 after complete dissolution, and mixing the copper nitrate solution with the pure water according to the ratio of 0.8 mL: adding 0.5% polysorbate 80 solution into 100mL of copper nitrate solution, and shaking up to constant volume to obtain a solution to be detected;
(3) And (3) sequentially sampling, on-machine detection and data processing the solution to be detected in the step (2) to obtain the granularity of the copper alloy.
The machine-up detection process in this example used a Bettersize C400 optical particle counter.
Example 3
The present embodiment provides an analysis method for counting particles of copper or copper alloy, the analysis method comprising the steps of:
(1) Preparing a copper alloy with the purity of more than or equal to 99.9999wt% into a columnar sample with the size specification of phi 3 x 5mm, and washing the copper alloy after sample preparation for 4.5min by using dilute nitric acid with the volume ratio of the nitric acid to the pure water of 1:1, wherein the concentration of the nitric acid is 66.5wt%, so as to obtain the pretreated copper alloy;
(2) Mixing nitric acid and pure water according to the volume ratio of 0.9 to 1 to obtain an etching solution, mixing the copper alloy pretreated in the step (1) and the etching solution according to the volume ratio of 0.12g to 1mL, dissolving a sample in a reaction vessel at normal temperature for 2.0h, neutralizing the copper nitrate solution with ammonium hydroxide to pH =7 after complete dissolution, and mixing the copper nitrate solution with the copper alloy and the etching solution according to the ratio of 1.2 mL: adding 0.9% polysorbate 20 solution into 100mL of copper nitrate solution, and shaking up to constant volume to obtain a solution to be detected;
(3) And (3) sequentially sampling, on-machine detection and data processing the solution to be detected in the step (2) to obtain the granularity of the copper alloy.
The machine-up detection process used in this example was a model Bettersize C400 optical particle counter.
Example 4
This example provides an analytical method for counting fine particles of copper or a copper alloy, which differs from example 1 only in that the volume ratio of nitric acid to pure water in the mixed acid of step (2) is 0.9.
Example 5
This example provides an analytical method for counting fine particles of copper or a copper alloy, which differs from example 1 only in that the volume ratio of nitric acid to pure water in the mixed acid of step (2) is 1.0.
Example 6
This example provides an analytical method for counting particles of copper or copper alloy, which differs from example 1 only in that the sample dissolution temperature in step (2) is 23 ℃, and the rest is the same as example 1.
Example 7
This example provides an analytical method for counting particles of copper or copper alloy, which differs from example 1 only in that the sample dissolution temperature in step (2) is 24 ℃, and the rest is the same as example 1.
Comparative example 1
This comparative example provides an analytical method for counting particles of copper or copper alloy, which differs from example 1 only in that the sample dissolution temperature in step (2) is 100 ℃, and the rest is the same as example 1.
Comparative example 2
This comparative example provides an analytical method for counting particles of copper or copper alloy, which differs from example 1 only in that the volume ratio of nitric acid and pure water in the mixed acid of step (2) is 2:1, and the rest is the same as example 1.
Comparative example 3
This comparative example provides an analytical method for counting fine particles of copper or copper alloy, which differs from example 1 only in that in step (1) copper or copper alloy is a chip-like sample having a thickness of 2mm and a length of 1cm, and the rest is the same as example 1.
Comparative example 4
This comparative example provides an analytical method for counting copper or copper alloy particles, which differs from example 1 only in that step (2) is not subjected to the alkali agent neutralization test, and the rest is the same as example 1.
Comparative example 5
This comparative example provides an analytical method for counting copper or copper alloy particles, which differs from example 1 only in that the mixed acid of step (2) is replaced with concentrated hydrochloric acid, and the rest is the same as example 1.
Comparative example 6
The present comparative example provides an analysis method for counting particles of copper or copper alloy, which differs from example 1 only in that the volume ratio of nitric acid and pure water in the mixed acid of step (2) is 0.5.
In comparative examples 5 to 6, the dissolution rate of copper or copper alloy exceeded 24 hours, and the particle counting process was not performed.
3. Test and results
The testing method of RSD comprises the following steps: the relative RSD was calculated by performing 3 particle counts of copper or copper alloy.
The test results of the above examples and comparative examples are shown in table 1.
TABLE 1 test results of examples and comparative examples
From table 1, the following points can be seen:
(1) The invention provides an analysis method for counting particles of copper or copper alloy, which fixes the sampling method and the state of a sample, reduces the surface pollution of the sample, controls the concentration of corrosive liquid and the sample dissolving temperature, thereby controlling the reaction speed, stabilizing the sample dissolving time, slowly dissolving the sample and preventing impurities from dissolving; the solution prepared by the analysis method is a neutral solution, so that the stability of the state of particles in the solution is improved, the data is more stable, and the acid and alkali resistance selection of equipment is more friendly.
(2) As can be seen from the combination of example 1 and examples 4 to 5, the volume ratio of nitric acid to pure water in the mixed acid of step (2) in example 1 is 0.8;
(3) It can be seen from the combination of examples 1 and 6 to 7 that the sample dissolution temperature of step (2) in example 1 was 25 ℃, the sample dissolution time of example 1 was 2.5h, and the RSD of the test result data was 10.0, compared to the sample dissolution temperatures of step (2) in examples 6 to 7, which were 23 ℃ and 24 ℃, respectively, whereas the RSD of examples 6 to 7 were 2.5h and 2.5h, respectively, and the RSD of the test result data was 9.6 and 8.9, respectively, thereby showing that a slight change in temperature did not significantly affect the results as long as the samples were dissolved at normal temperature;
(4) By combining example 5 and comparative example 1, it can be seen that the sample dissolution temperature of step (2) in example 1 is 25 ℃, compared with the sample dissolution temperature of step (2) in comparative example 1 being 100 ℃, the sample dissolution time of example 1 is 1h, the RSD of the test result data is 3.7, the sample dissolution time of comparative example 1 is 35min, and the RSD of the test result data is 5.4, thereby showing that the present invention stabilizes the sample dissolution temperature, controls the reaction speed and the sample dissolution time, slowly dissolves the sample, prevents the dissolution of impurities, and makes the data more stable;
(5) As can be seen by combining example 1 and comparative example 2, the volume ratio of nitric acid to pure water in the mixed acid of step (2) in example 1 is 0.8;
(6) It can be known from the combination of the example 1 and the comparative example 3 that the copper or copper alloy of the step (1) in the example 1 is a columnar sample with the size specification of phi 5 x 5mm, compared with the copper or copper alloy of the step (1) in the comparative example 3 which is a chip sample with the thickness of 2mm and the length of 1cm, the sample of the example 1 has the dissolution time of 2.5h, the RSD of the test result data is 10.0, while the sample of the comparative example 3 has the dissolution time of 15min, and the RSD of the test result data is 26.6, thereby showing that the invention clearly determines the sampling specification and state, is beneficial to reducing the surface pollution of the sample, controls the reaction speed, stabilizes the sample dissolution time to slowly dissolve the sample, prevents the dissolution of impurities, and makes the data more stable;
(7) By combining the example 1 and the comparative example 4, the experiment of neutralizing the alkaline agent and adding the surfactant is carried out in the step (2) in the example 1, compared with the experiment of not carrying out the neutralization of the alkaline agent and adding the surfactant in the step (2) in the comparative example 4, the dissolution time of the sample in the example 1 is 2.5h, the RSD of the test result data is 10.0, the dissolution time of the sample in the comparative example 4 is 2.5h, the RSD of the test result data is 16, and the RSD of the test data after the sample is placed for 20min and the RSD of the original test data are 1.2 and 4.9 respectively, so that the invention can obtain more stable data by neutralizing and adding the surfactant in the alkaline agent and is friendly to the acid and alkali resistance requirements of equipment;
(8) Combining example 1 with comparative examples 5 and 6, it can be seen that the volume ratio of nitric acid and pure water in the step (2) mixed acid in example 1 is 0.8.
In summary, the invention provides an analysis method for improving the particle counting stability in a copper nitrate solution, which is characterized in that the analysis method comprises the steps of pretreating copper or a copper alloy, dissolving the pretreated copper or copper alloy in a prepared corrosive liquid to obtain a copper nitrate solution, neutralizing the copper nitrate solution with an alkaline reagent until the pH is =7, adding a surfactant, and carrying out constant volume shaking to obtain a solution to be measured; and then analyzing and calculating the granularity of the copper or copper alloy material in the solution to be detected, wherein the solution prepared by the analysis method is a neutral solution, so that the stability of the state of the particles in the solution is improved, the data are more stable, the selection of acid and alkali resistance of equipment is more friendly, the dissolving time of the copper or copper alloy is less than or equal to 2.5 hours and the relative standard deviation is less than or equal to 10.0 under the optimal condition.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. An analytical method for particle counting of copper or copper alloys comprising the steps of:
(1) Sampling copper or copper alloy to obtain a copper or copper alloy sample, and then pretreating the copper or copper alloy sample;
(2) Preparing a corrosive liquid by using nitric acid and pure water according to the volume ratio of (0.6-1.2) to 1;
(3) Dissolving a copper or copper alloy sample in a corrosive liquid to obtain a copper nitrate solution; the proportion of the copper or copper alloy sample to the corrosive liquid is (0.08-0.12) g:1mL;
(4) Adjusting the pH of the copper nitrate solution to =7 by using an alkaline reagent, then adding a surfactant into the solution, and performing constant volume shaking to obtain a solution to be detected;
(5) And detecting the number of particles in the liquid to be detected.
2. The method as claimed in claim 1, wherein the purity of the copper or copper alloy in step (1) is 99.9999wt%.
3. The method according to claim 1, wherein the copper or copper alloy sample in step (1) is a columnar sample.
4. The method of claim 3, wherein the columnar sample has a gauge of 2mm to 5mm by 5mm.
5. The method for analyzing particle count of copper or copper alloy according to claim 1, wherein the pretreatment in step (1) is: and washing the copper or copper alloy sample by using dilute nitric acid for 3-5min.
6. The method of claim 1, wherein the nitric acid concentration in step (2) is 65 to 68wt%.
7. The method of claim 1, wherein the dissolution time in step (3) is 1-2.5 hours.
8. The method of claim 1, wherein the alkaline reagent used in step (4) is electronic grade triethanolamine or ammonium hydroxide.
9. The method of claim 1, wherein the surfactant in step (4) is one or more of polysorbate 20, polysorbate 80, or Triton X-100.
10. The method of claim 1, wherein the surfactant is present in the amount of 0.05-1% in step (4); the ratio of surfactant to copper nitrate solution was (0.8-1.2) mL:100mL.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106706605A (en) * | 2016-12-27 | 2017-05-24 | 武汉泛洲中越合金有限公司 | Method for detecting content of chromium in copper alloy |
| US20190293541A1 (en) * | 2016-12-15 | 2019-09-26 | Denso Corporation | Particulate matter detection apparatus |
| CN111751251A (en) * | 2020-07-01 | 2020-10-09 | 宁波江丰电子材料股份有限公司 | Test method of high-purity aluminum alloy |
| CN113252645A (en) * | 2021-04-30 | 2021-08-13 | 宁波金田铜业(集团)股份有限公司 | Method for rapidly determining chromium content in copper or copper alloy |
| CN113295493A (en) * | 2021-05-24 | 2021-08-24 | 宁波江丰电子材料股份有限公司 | Sample preparation method for counting particles of high-purity titanium |
| CN114136849A (en) * | 2021-11-24 | 2022-03-04 | 蜂巢能源科技有限公司 | Granularity test method of ternary cathode material |
-
2023
- 2023-01-10 CN CN202310036978.2A patent/CN115753567A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190293541A1 (en) * | 2016-12-15 | 2019-09-26 | Denso Corporation | Particulate matter detection apparatus |
| CN106706605A (en) * | 2016-12-27 | 2017-05-24 | 武汉泛洲中越合金有限公司 | Method for detecting content of chromium in copper alloy |
| CN111751251A (en) * | 2020-07-01 | 2020-10-09 | 宁波江丰电子材料股份有限公司 | Test method of high-purity aluminum alloy |
| CN113252645A (en) * | 2021-04-30 | 2021-08-13 | 宁波金田铜业(集团)股份有限公司 | Method for rapidly determining chromium content in copper or copper alloy |
| CN113295493A (en) * | 2021-05-24 | 2021-08-24 | 宁波江丰电子材料股份有限公司 | Sample preparation method for counting particles of high-purity titanium |
| CN114136849A (en) * | 2021-11-24 | 2022-03-04 | 蜂巢能源科技有限公司 | Granularity test method of ternary cathode material |
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