CN111751251A - Test method of high-purity aluminum alloy - Google Patents
Test method of high-purity aluminum alloy Download PDFInfo
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- CN111751251A CN111751251A CN202010626737.XA CN202010626737A CN111751251A CN 111751251 A CN111751251 A CN 111751251A CN 202010626737 A CN202010626737 A CN 202010626737A CN 111751251 A CN111751251 A CN 111751251A
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 53
- 238000010998 test method Methods 0.000 title claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 98
- 239000000523 sample Substances 0.000 claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000007788 liquid Substances 0.000 claims abstract description 54
- 239000000243 solution Substances 0.000 claims abstract description 42
- 239000002245 particle Substances 0.000 claims abstract description 37
- 239000012488 sample solution Substances 0.000 claims abstract description 35
- 238000005260 corrosion Methods 0.000 claims abstract description 28
- 230000007797 corrosion Effects 0.000 claims abstract description 27
- 238000005303 weighing Methods 0.000 claims abstract description 13
- 238000010790 dilution Methods 0.000 claims abstract description 12
- 239000012895 dilution Substances 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 238000010008 shearing Methods 0.000 claims abstract description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 28
- 238000005554 pickling Methods 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 9
- 238000005530 etching Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 238000001514 detection method Methods 0.000 abstract description 14
- 238000012360 testing method Methods 0.000 abstract description 14
- 239000003792 electrolyte Substances 0.000 description 6
- 238000009713 electroplating Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- WPPDFTBPZNZZRP-UHFFFAOYSA-N aluminum copper Chemical compound [Al].[Cu] WPPDFTBPZNZZRP-UHFFFAOYSA-N 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002997 ophthalmic solution Substances 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
Abstract
The invention discloses a method for testing high-purity aluminum alloy. The test method of the high-purity aluminum alloy comprises the following steps: 1) shearing a high-purity aluminum alloy sample, and carrying out impurity removal pretreatment; 2) weighing a pretreated high-purity aluminum alloy sample, adding a corrosive liquid for corrosion, standing, and adding water for dilution to form a mixed sample liquid; 3) weighing the mixed sample solution, adding water for dilution, detecting the granularity of the sample solution by a liquid particle counter, detecting for at least 3 times, and taking an average value S1; 4) adding water into hydrochloric acid to form a hydrochloric acid solution in the same proportion as the mixed sample liquid in the step 3), taking the hydrochloric acid solution, adding water for dilution, detecting by a liquid particle counter, detecting for at least 3 times, taking an average value S2, and calculating the particle size of the sample. The testing method of the high-purity aluminum alloy shortens the corrosion time of a high-purity aluminum alloy sample, improves the detection efficiency, reduces the possibility of sample liquid pollution, and makes the data more stable.
Description
Technical Field
The invention relates to the technical field of alloy sample preparation, relates to a test method of high-purity aluminum alloy, and particularly relates to an LPC test method of high-purity aluminum alloy.
Background
Liquid Particle Counters (LPC) are a device for determining the number of particles in suspension and the particle size distribution in liquids, and are outstanding in quality control and research applications in the field of particle counting. CN104005078A discloses an electroplating apparatus for electroplating metal onto a semiconductor wafer, which may comprise an electroplating bath, an electrolyte circulation system connected to the bath for circulating electrolyte to and from the bath, first and second sampling ports for taking first and second samples of electrolyte at first and second locations in the apparatus, and one or more liquid particle counter modules connected to the first and second sampling ports for measuring the concentration of particles in the electrolyte.
It also discloses a method for reducing the concentration of particles in an electrolyte present in an electroplating apparatus, which may include determining an approximate particle concentration using a liquid particle counter module, and adjusting operation of the electroplating apparatus to reduce the concentration of particles in the electrolyte. When particles in the liquid pass through a narrow detection zone, the sensor output signal changes due to being blocked by insoluble particles. According to the principle, the LPC can accurately detect the number of particles in the sample to be detected. The detection is accurate, the flow rate is controllable, the sample volume in the whole range can be processed, and the accurate measurement can be realized from 1 ml to more than 1000 ml; the detection range is wide, and the sample detection with the smallest particle size range from 0.5 mu m to 600 mu m is realized through the interchangeable sensor; meanwhile, LPC is simple to operate and convenient to sample, and is widely applied to the fields of scientific research and test of pharmaceutical grades and detection of insoluble substances in metals.
The test method of the high-purity aluminum alloy is as follows: turning a high-purity aluminum target into a filamentous sample, dissolving the sample in hydrochloric acid through the steps of acid washing, corrosion and the like to form a mixed sample solution, detecting the granularity of the sample solution by LPC, and calculating to obtain a final result.
The test method in the prior art is as follows: sample pretreatment (shearing-pickling-drying) -corrosion (hydrochloric acid) -sampling-instrument detection-data processing. However, the testing method in the prior art has the disadvantages of long corrosion time (15h) of high-purity aluminum alloy, long sample testing period and low efficiency.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for testing high-purity aluminum alloy, which shortens the corrosion time of a high-purity aluminum alloy sample, improves the detection efficiency, reduces the possibility of sample liquid pollution and enables data to be more stable.
In order to achieve the purpose, the invention adopts the following technical scheme:
a test method of high-purity aluminum alloy comprises the following steps:
1) shearing a high-purity aluminum alloy sample, and carrying out impurity removal pretreatment;
2) weighing a pretreated high-purity aluminum alloy sample, adding a corrosive liquid for corrosion, standing, and adding water for dilution to form a mixed sample liquid; wherein the corrosive liquid is a mixed liquid of hydrochloric acid and water, and the volume ratio of the hydrochloric acid to the water is (2.5-3.5) to (2.5-3.5);
3) weighing the mixed sample solution, adding water for dilution, detecting the granularity of the sample solution by a liquid particle counter, detecting for at least 3 times, and taking an average value S1;
4) adding water into hydrochloric acid to form a hydrochloric acid solution, wherein the volume ratio of the hydrochloric acid to the water is (2.5-3.5) - (2.5-3.5), taking the hydrochloric acid solution, adding water to dilute the hydrochloric acid solution, detecting the hydrochloric acid solution by using a liquid particle counter, detecting for at least 3 times, taking an average value S2, and calculating the granularity of the sample by using S1 and S2.
According to the method for testing the high-purity aluminum alloy, impurities of the high-purity aluminum alloy sample are removed through pretreatment, the mixed sample liquid is prepared after corrosion by adding the corrosive liquid, the corrosion time of the high-purity aluminum alloy sample is shortened, the detection efficiency is improved, the possibility of sample liquid pollution is reduced, and the data are more stable.
The calculation formula of the sample granularity in the invention is (S1-S2) multiplied by 1000/M, wherein M is the mass of the high-purity aluminum alloy sample before corrosion.
In the step 1), the high-purity aluminum alloy is 5N high-purity aluminum alloy. It should be noted that the 5N high purity aluminum alloy means an aluminum alloy having a purity of 99.999%, i.e., the total content of impurity elements other than the alloying elements is not more than 0.001%, for example, a 5N high purity aluminum copper alloy means the total content of impurity elements other than aluminum copper is not more than 0.001%.
In the step 1), the impurity removal pretreatment is drying after acid washing.
Preferably, the volume of the pickling solution used for pickling the mass of 1.5g to 2.5g of the high-purity aluminum alloy sample is 150 to 250 mL.
In the step 1), the pickling time is 2-4 min; for example, the time for pickling is 2min, 2.5min, 3min, 3.5min or 4 min.
Preferably, the pickling solution for pickling is a mixed acid of nitric acid and hydrofluoric acid;
preferably, the volume ratio of the nitric acid to the hydrofluoric acid to the water is (3.5-4.5): (0.5-1.5): (0.5-1.5).
In the step 2), the volume of the corrosive liquid used by 1.5 g-2.5 g of the high-purity aluminum alloy sample is 150-250 mL.
In the step 2), the corrosive liquid is a mixed liquid of hydrochloric acid and water.
Preferably, the etching time is 4.5h to 7h, for example, the etching time is 4h, 4.5h, 5h, 5.5h, 6h, 6.5h or 7 h.
In the step 2), heating treatment is carried out in the corrosion process of the corrosive liquid; preferably, the heating temperature is 40 to 45 ℃, for example, the heating temperature is 40 ℃, 41 ℃, 42 ℃, 43 ℃, 44 ℃ or 45 ℃.
In the step 2), the mass of water used for diluting with water is 35-45 mL.
In the step 3), the volume ratio of the mixed sample liquid to the water is (0.5-1.5) to (8.5-9.5).
In the step 4), when water is added for dilution, the volume ratio of the hydrochloric acid solution to the water is (0.5-1.5) to (8.5-9.5).
The invention shortens the corrosion time and further shortens the sample measuring period by reducing the sampling amount and improving the proportion of the hydrochloric acid and the water during corrosion.
The high purity aluminum alloy prepared by the test method of the invention can be used for insoluble particles in ophthalmic solutions, sterile pharmaceutical preparations, injections and liquid for injection.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for testing the high-purity aluminum alloy, impurities of the high-purity aluminum alloy sample are removed through pretreatment, the mixed sample liquid is prepared after corrosion of the high-purity aluminum alloy sample is carried out by adding the corrosive liquid, the corrosion time of the high-purity aluminum alloy sample is shortened, the corrosion can be completed within 4.5-7 h, the detection efficiency is improved, the detection precision is 99.9%, the detection efficiency is 99.9%, the possibility of pollution of the sample liquid is reduced, and the data are more stable.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Unless otherwise specified, various starting materials of the present invention are commercially available or prepared according to conventional methods in the art.
The test method of the high-purity aluminum alloy comprises the following steps:
1) shearing a high-purity aluminum alloy sample, and carrying out impurity removal pretreatment;
2) weighing a pretreated high-purity aluminum alloy sample, adding a corrosive liquid for corrosion, standing, and adding water for dilution to form a mixed sample liquid; wherein the corrosive liquid is a mixed liquid of hydrochloric acid and water;
3) weighing the mixed sample solution, adding water for dilution, detecting the granularity of the sample solution by a liquid particle counter, detecting for at least 3 times, and taking an average value S1;
4) adding water into hydrochloric acid to form a hydrochloric acid solution in the same proportion as the mixed sample liquid in the step 3), taking the hydrochloric acid solution, adding water for dilution, detecting by a liquid particle counter, detecting for at least 3 times, taking an average value S2, and calculating the particle size of the sample by utilizing S1 and S2.
The particle size is calculated as follows:
the particle size was (S1-S2) × 1000/M,
wherein M is the mass of the high-purity aluminum alloy sample before corrosion.
Example 1
The method for testing the high-purity aluminum alloy comprises the following steps:
1) shearing a 5N high-purity aluminum alloy sample, taking 10g of the sample, and mixing the volume ratio of each component in a mixed acid solution of nitric acid and hydrofluoric acid with the following components: nitric acid: hydrofluoric acid: pickling with water at a ratio of 4:1:1 for 3min, and drying under a big sun lamp;
2) weighing 1.8g of sample, adding 30mL of hydrochloric acid and 30mL of pure water for corrosion, standing for 5 hours, then enabling the solution to be transparent and clear, and adding 40mL of pure water to finally form a mixed sample solution;
3) taking 10mL of mixed sample solution, adding 90mL of pure water, detecting the granularity of the sample solution by a liquid particle counter, repeating the steps for more than three times in parallel, and taking an average value S1;
4) adding 70mL of pure water into 30mL of hydrochloric acid to form a hydrochloric acid solution in the same proportion as the mixed sample solution, taking 10mL of hydrochloric acid solution, adding 90mL of pure water, detecting the granularity of the sample solution by a liquid particle counter, taking an average value S2 in parallel three times, and calculating the granularity of the sample by using a formula.
Example 2
The method for testing the high-purity aluminum alloy comprises the following steps:
1) shearing a 5N high-purity aluminum alloy sample, taking 10g of the sample, and mixing the volume ratio of each component in a mixed acid solution of nitric acid and hydrofluoric acid with the following components: nitric acid: hydrofluoric acid: pickling with water at a ratio of 4:1:1 for 3min, and drying under a big sun lamp;
2) weighing 1.9g of sample, adding 30mL of hydrochloric acid and 30mL of pure water for corrosion, standing for 6 hours, then enabling the solution to be transparent and clear, and adding 40mL of pure water to finally form a mixed sample solution;
3) taking 10mL of mixed sample solution, adding 90mL of pure water, detecting the granularity of the sample solution by a liquid particle counter, repeating the steps for more than three times in parallel, and taking an average value S1;
4) adding 70mL of pure water into 30mL of hydrochloric acid to form a hydrochloric acid solution in the same proportion as the mixed sample solution, taking 10mL of hydrochloric acid solution, adding 90mL of pure water, detecting the granularity of the sample solution by a liquid particle counter, taking an average value S2 in parallel three times, and calculating the granularity of the sample by using a formula.
Example 3
The method for testing the high-purity aluminum alloy comprises the following steps:
1) shearing a 5N high-purity aluminum alloy sample, taking 10g of the sample, and mixing the following components in nitric acid and hydrofluoric acid according to the volume ratio: nitric acid: hydrofluoric acid: pickling with water at a ratio of 4:1:1 for 3min, and drying under a big sun lamp;
2) weighing 2g of sample, adding 30mL of hydrochloric acid and 30mL of pure water for corrosion, standing for 6.5h, then enabling the solution to be transparent and clear, and adding 40mL of pure water to finally form a mixed sample solution;
3) taking 10mL of mixed sample solution, adding 90mL of pure water, detecting the granularity of the sample solution by a liquid particle counter, repeating the steps for more than three times in parallel, and taking an average value S1;
4) adding 70mL of pure water into 30mL of hydrochloric acid to form a hydrochloric acid solution in the same proportion as the mixed sample solution, taking 10mL of hydrochloric acid solution, adding 90mL of pure water, detecting the granularity of the sample solution by a liquid particle counter, taking an average value S2 in parallel three times, and calculating the granularity of the sample by using a formula.
Example 4
The method for testing the high-purity aluminum alloy comprises the following steps:
1) shearing a 5N high-purity aluminum alloy sample, taking 10g of the sample, and mixing the volume ratio of each component in a mixed acid solution of nitric acid and hydrofluoric acid with the following components: nitric acid: hydrofluoric acid: pickling with water at a ratio of 4:1:1 for 3min, and drying under a big sun lamp;
2) weighing 2.2g of sample, adding 30mL of hydrochloric acid and 30mL of pure water for corrosion, standing for 7 hours, then obtaining a transparent and clear solution, and adding 40mL of pure water to finally form a mixed sample solution;
3) taking 10mL of mixed sample solution, adding 90mL of pure water, detecting the granularity of the sample solution by a liquid particle counter, repeating the steps for more than three times in parallel, and taking an average value S1;
4) adding 70mL of pure water into 30mL of hydrochloric acid to form a hydrochloric acid solution in the same proportion as the mixed sample solution, taking 10mL of hydrochloric acid solution, adding 90mL of pure water, detecting the granularity of the sample solution by a liquid particle counter, taking an average value S2 in parallel three times, and calculating the granularity of the sample by using a formula.
Example 5
The difference between this example and example 1 is that in step 2), the etching solution was subjected to a heat treatment at 45 ℃ during etching, and the etching time was 3.5 hours, which is otherwise the same as that of example 1.
Example 6
The method for testing the high-purity aluminum alloy comprises the following steps:
1) shearing a 5N high-purity aluminum alloy sample, taking 10g of the sample, and mixing the volume ratio of each component in a mixed acid solution of nitric acid and hydrofluoric acid with the following components: nitric acid: hydrofluoric acid: pickling with water at a ratio of 4:1:1 for 3min, and drying under a big sun lamp;
2) weighing 4g of sample, adding 30mL of hydrochloric acid and 30mL of pure water for corrosion, standing for 15h, then enabling the solution to be transparent and clear, and adding 40mL of pure water to finally form a mixed sample solution;
3) taking 10mL of mixed sample solution, adding 90mL of pure water, detecting the granularity of the sample solution by a liquid particle counter, repeating the steps for more than three times in parallel, and taking an average value S1;
4) adding 70mL of pure water into 30mL of hydrochloric acid to form a hydrochloric acid solution in the same proportion as the mixed sample solution, taking 10mL of hydrochloric acid solution, adding 90mL of pure water, detecting the granularity of the sample solution by a liquid particle counter, taking an average value S2 in parallel three times, and calculating the granularity of the sample by using a formula.
Compared with the embodiment 1, the heat treatment can shorten the etching time in the etching of the embodiment 5; comparing the embodiment 1 with the embodiment 6, the testing method can finish corrosion within 4.5-7 h, improves the detection efficiency, has 99.9% of detection precision and 99.9% of detection efficiency, and needs 15h of corrosion time of the embodiment 6 in order to achieve the effect of the application.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The test method of the high-purity aluminum alloy is characterized by comprising the following steps:
1) shearing a high-purity aluminum alloy sample, and carrying out impurity removal pretreatment;
2) weighing a pretreated high-purity aluminum alloy sample, adding a corrosive liquid for corrosion, standing, and adding water for dilution to form a mixed sample liquid; wherein the corrosive liquid is a mixed liquid of hydrochloric acid and water, and the volume ratio of the hydrochloric acid to the water is (2.5-3.5) to (2.5-3.5);
3) weighing the mixed sample solution, adding water for dilution, detecting the granularity of the sample solution by a liquid particle counter, detecting for at least 3 times, and taking an average value S1;
4) adding water into hydrochloric acid to form a hydrochloric acid solution, wherein the volume ratio of the hydrochloric acid to the water is (2.5-3.5) - (2.5-3.5), taking the hydrochloric acid solution, adding water to dilute the hydrochloric acid solution, detecting the hydrochloric acid solution by using a liquid particle counter, detecting for at least 3 times, taking an average value S2, and calculating the granularity of the sample by using S1 and S2.
2. The test method as claimed in claim 1, wherein in step 1), the high purity aluminum alloy is a 5N high purity aluminum alloy.
3. The test method according to claim 1 or 2, wherein in the step 1), the impurity removal pretreatment is drying after acid washing;
preferably, the volume of the pickling solution used for pickling the mass of 1.5g to 2.5g of the high-purity aluminum alloy sample is 150 to 250 mL.
4. The test method according to claim 3, wherein in the step 1), the acid washing time is 2-4 min;
preferably, the pickling solution for pickling is a mixed solution of nitric acid, hydrofluoric acid and water;
preferably, the volume ratio of the nitric acid to the hydrofluoric acid to the water is (3.5-4.5): (0.5-1.5): (0.5-1.5).
5. The test method according to any one of claims 1 to 4, wherein in the step 2), the volume of the etching solution used for 1.5g to 2.5g of the high purity aluminum alloy sample is 150 to 250 mL.
6. The test method according to any one of claims 1 to 5, wherein the etching time in step 2) is 4.5 to 7 hours.
7. The test method according to one of claims 1 to 6, wherein in the step 2), the corrosion solution is heated during corrosion;
preferably, the heating temperature is 40-45 ℃.
8. The test method according to any one of claims 1 to 7, wherein the volume of water used for water dilution in step 2) is 35 to 45 mL.
9. The test method according to any one of claims 1 to 8, wherein in the step 3), the volume ratio of the mixed sample liquid to the water is (0.5 to 1.5): (8.5 to 9.5).
10. The test method according to any one of claims 1 to 9, wherein in the step 4), the volume ratio of the hydrochloric acid solution to the water when diluted with water is (0.5 to 1.5): (8.5 to 9.5).
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| CN202010626737.XA CN111751251A (en) | 2020-07-01 | 2020-07-01 | Test method of high-purity aluminum alloy |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111751254A (en) * | 2020-07-13 | 2020-10-09 | 宁波江丰电子材料股份有限公司 | Method for testing granularity of high-purity aluminum alloy sample |
| 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 |
| CN115753567A (en) * | 2023-01-10 | 2023-03-07 | 有研亿金新材料有限公司 | Analysis method for counting particles of copper or copper alloy |
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