CN111751254A - Method for testing granularity of high-purity aluminum alloy sample - Google Patents
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 59
- 238000012360 testing method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 89
- 239000007788 liquid Substances 0.000 claims abstract description 82
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000002245 particle Substances 0.000 claims abstract description 48
- 239000002253 acid Substances 0.000 claims abstract description 43
- 238000005260 corrosion Methods 0.000 claims abstract description 40
- 230000007797 corrosion Effects 0.000 claims abstract description 40
- 239000011259 mixed solution Substances 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 19
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 48
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 25
- 229910017604 nitric acid Inorganic materials 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 21
- 238000005554 pickling Methods 0.000 claims description 20
- 238000010008 shearing Methods 0.000 claims description 11
- 238000010998 test method Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000005530 etching Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 36
- 238000013461 design Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 8
- 239000003792 electrolyte Substances 0.000 description 6
- 238000009713 electroplating Methods 0.000 description 5
- 238000007792 addition Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000004065 semiconductor 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
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- G—PHYSICS
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- 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
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- 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
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- 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
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- 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
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- 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
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- 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
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Abstract
The invention relates to a method for testing the granularity of a high-purity aluminum alloy sample, which comprises the following steps: (1) mixing a sample liquid obtained after the high-purity aluminum alloy sample is corroded with water, detecting for at least 3 times by using a liquid particle counter, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water; (2) mixing acid solution used in corrosion with water, detecting at least 3 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of the sample by using S1 and S2. The testing method provided by the invention realizes the detection of the high-purity aluminum alloy sample by using the liquid particle counter through the reasonable design of the testing steps, and meanwhile, the detection precision and efficiency are also obviously improved.
Description
Technical Field
The invention relates to the field of testing, relates to a method for testing granularity, and particularly relates to a method for testing the granularity of a high-purity aluminum alloy sample.
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.
However, the current liquid particle counter can only detect the particle size of the high-purity copper alloy in the metal detection industry, the sampling is single, the comparison is not obvious, and the reference value is low.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a method for testing the granularity of a high-purity aluminum alloy sample, and the method provided by the invention realizes the detection of the high-purity aluminum alloy sample by using a liquid particle counter, and obviously improves the detection precision and efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for testing the granularity of a high-purity aluminum alloy sample, which comprises the following steps:
(1) mixing a sample liquid obtained after the high-purity aluminum alloy sample is corroded with water, detecting for at least 3 times by using a liquid particle counter, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water;
(2) mixing acid solution used in corrosion with water, detecting at least 3 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of the sample by using S1 and S2.
The testing method provided by the invention realizes the detection of the high-purity aluminum alloy sample by using the liquid particle counter through the reasonable design of the testing steps, and meanwhile, the detection precision and efficiency are also obviously improved.
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 (not less than 3N) before corrosion.
As a preferable technical scheme of the invention, the high-purity aluminum alloy sample in the step (1) is sequentially sheared, pickled and dried before being corroded.
In a preferred embodiment of the present invention, the maximum length of the high purity aluminum alloy sample after shearing is 1 to 3cm, for example, 1cm, 1.2cm, 1.4cm, 1.6cm, 1.8cm, 2cm, 2.2cm, 2.4cm, 2.6cm, 2.8cm or 3cm, but is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
In a preferred embodiment of the present invention, the acid washing time is 2 to 5min, and may be, for example, 2min, 2.5min, 3min, 3.5min, 4min, 4.5min, or 5min, but is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
In a preferred embodiment of the present invention, the washing liquid used in the pickling is a mixed liquid of nitric acid, hydrofluoric acid, and water.
In a preferred embodiment of the present invention, the volume ratio of nitric acid, hydrofluoric acid and water in the mixed solution is (3-5): (0.5-1.5): (0.5-1.5), and examples thereof include 3:0.5:0.5, 3:1.5:0.5, 3:0.5:1.5, 3:1:0.5, 3:0.5:1, 4:0.5:0.5, 5:0.5:0.5 or 4:1:1, but are not limited to the above-mentioned values, and other values not listed in this range are also applicable.
In a preferred embodiment of the present invention, the volume ratio of hydrochloric acid to water in the mixed solution is (0.5-0.7):1, and may be, for example, 0.5:1, 0.55:1, 0.6:1, 0.65:1, or 0.7:1, but is not limited to the above-mentioned values, and other values not mentioned in the above range are also applicable.
Preferably, the etching time is 14 to 17 hours, for example, 14 hours, 14.5 hours, 15 hours, 15.5 hours, 16 hours, 16.5 hours, or 17 hours, etc., but not limited to the recited values, and other values not recited in the range are also applicable.
As a preferred embodiment of the present invention, the volume ratio of the sample liquid and water in step (1) is (0.5-1.5): (8.5-9.5), and may be, for example, 0.5:8.5, 0.5:9, 0.5:9.5, 1:8.5, 1.5:8.5, 1:9, 1.5:9, 1:9.5 or 1.5:9.5, but not limited to the values listed, and other values not listed in this range are also applicable.
In a preferred embodiment of the present invention, the volume ratio of the acid solution to the water in the step (2) is (0.5-1.5): (8.5-9.5), and may be, for example, 0.5:8.5, 0.5:9, 0.5:9.5, 1:8.5, 1.5:8.5, 1:9, 1.5:9, 1:9.5 or 1.5:9.5, but not limited to the above-mentioned values, and other values not listed in this range are also applicable.
As a preferred technical solution of the present invention, the test method includes:
(1) mixing a sample liquid obtained after the high-purity aluminum alloy sample is corroded with water, detecting for at least 3 times by using a liquid particle counter, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water; shearing, pickling and drying the high-purity aluminum alloy sample in sequence before corrosion; the maximum length of the high-purity aluminum alloy sample after being cut into pieces is 1-3 cm; the pickling time is 2-5 min; the washing liquid in the acid washing is a mixed liquid of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid, hydrofluoric acid and water in the mixed solution is (3-5) to (0.5-1.5); the volume ratio of the hydrochloric acid to the water in the mixed solution is (0.5-0.7) to 1; the corrosion time is 14-17 h; the volume ratio of the sample liquid to the water is (0.5-1.5) to (8.5-9.5);
(2) mixing acid liquor used in corrosion with water, detecting for at least 3 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of a sample by using S1 and S2; wherein the volume ratio of the acid liquid to the water is (0.5-1.5) to (8.5-9.5).
Compared with the prior art, the invention at least has the following beneficial effects:
the testing method provided by the invention realizes the detection of the particle size distribution and the size of the high-purity aluminum alloy sample by using the liquid particle counter through the reasonable design of the testing steps, and simultaneously, the detection precision and the efficiency are also obviously improved, and the detection precision reaches more than 95%.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a method for testing the granularity of a high-purity aluminum alloy sample, which comprises the following steps:
(1) mixing a sample liquid obtained by corroding a high-purity aluminum alloy sample (not less than 3N) with water, detecting for 3 times by using a liquid particle counter, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water; shearing, pickling and drying the high-purity aluminum alloy sample in sequence before corrosion; the maximum length of the high-purity aluminum alloy sample after being cut into pieces is 2 cm; the pickling time is 3 min; the washing liquid in the acid washing is a mixed liquid of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid, hydrofluoric acid and water in the mixed solution is 4:1: 1; the volume ratio of the hydrochloric acid to the water in the mixed solution is 1: 1; the corrosion time is 14 h; the volume ratio of the sample liquid to the water is 1.5: 9;
(2) mixing acid liquor used in corrosion with water, detecting for 3 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of a sample by using S1 and S2; wherein the volume ratio of the acid liquid to the water is 1:9.
The method realizes the detection of the grain size distribution and the size of the high-purity aluminum alloy sample, and the detection precision reaches 95 percent.
Example 2
The embodiment provides a method for testing the granularity of a high-purity aluminum alloy sample, which comprises the following steps:
(1) mixing a sample liquid obtained by corroding a high-purity aluminum alloy sample (not less than 3N) with water, detecting by using a liquid particle counter, detecting for 5 times, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water; shearing, pickling and drying the high-purity aluminum alloy sample in sequence before corrosion; the maximum length of the high-purity aluminum alloy sample after being cut into pieces is 1 cm; the pickling time is 5 min; the washing liquid in the acid washing is a mixed liquid of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid, hydrofluoric acid and water in the mixed solution is 3:1.5: 1; the volume ratio of the hydrochloric acid to the water in the mixed solution is 0.65: 1; the corrosion time is 17 h; the volume ratio of the sample liquid to the water is 0.5: 8.5;
(2) mixing acid liquor used in corrosion with water, detecting for 6 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of a sample by using S1 and S2; wherein the volume ratio of the acid liquid to the water is 1.5:9.
The method realizes the detection of the grain size distribution and the size of the high-purity aluminum alloy sample, and the detection precision reaches 96 percent.
Example 3
The embodiment provides a method for testing the granularity of a high-purity aluminum alloy sample, which comprises the following steps:
(1) mixing a sample liquid obtained by corroding a high-purity aluminum alloy sample (not less than 3N) with water, detecting for 6 times by using a liquid particle counter, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water; shearing, pickling and drying the high-purity aluminum alloy sample in sequence before corrosion; the maximum length of the high-purity aluminum alloy sample after being sheared into pieces is 1.3 cm; the pickling time is 4.7 min; the washing liquid in the acid washing is a mixed liquid of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid, hydrofluoric acid and water in the mixed solution is 5:0.5: 1.5; the volume ratio of the hydrochloric acid to the water in the mixed solution is 0.7: 1; the corrosion time is 15 h; the volume ratio of the sample liquid to the water is 1.2: 8.7;
(2) mixing acid liquor used in corrosion with water, detecting for 6 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of a sample by using S1 and S2; wherein the volume ratio of the acid liquid to the water is 0.7: 9.3.
The method realizes the detection of the grain size distribution and the size of the high-purity aluminum alloy sample, and the detection precision reaches 97 percent.
Example 4
The embodiment provides a method for testing the granularity of a high-purity aluminum alloy sample, which comprises the following steps:
(1) mixing a sample liquid obtained by corroding a high-purity aluminum alloy sample (not less than 3N) with water, detecting for 3 times by using a liquid particle counter, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water; shearing, pickling and drying the high-purity aluminum alloy sample in sequence before corrosion; the maximum length of the high-purity aluminum alloy sample after being sheared into pieces is 1.7 cm; the pickling time is 5 min; the washing liquid in the acid washing is a mixed liquid of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid to hydrofluoric acid to water in the mixed solution is 3.7:0.7: 1.2; the volume ratio of the hydrochloric acid to the water in the mixed solution is 0.67: 1; the corrosion time is 16 h; the volume ratio of the sample liquid to the water is 0.5: 8.5;
(2) mixing acid liquor used in corrosion with water, detecting for 3 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of a sample by using S1 and S2; wherein the volume ratio of the acid liquid to the water is 1.5: 9.5.
The method realizes the detection of the grain size distribution and the size of the high-purity aluminum alloy sample, and the detection precision reaches 95 percent.
Example 5
The embodiment provides a method for testing the granularity of a high-purity aluminum alloy sample, which comprises the following steps:
(1) mixing a sample liquid obtained by corroding a high-purity aluminum alloy sample (not less than 3N) with water, detecting for 3 times by using a liquid particle counter, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water; shearing, pickling and drying the high-purity aluminum alloy sample in sequence before corrosion; the maximum length of the high-purity aluminum alloy sample after being sheared into pieces is 2.8 cm; the pickling time is 2.7 min; the washing liquid in the acid washing is a mixed liquid of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid to hydrofluoric acid to water in the mixed solution is 4.7:1.5: 0.7; the volume ratio of the hydrochloric acid to the water in the mixed solution is 0.54: 1; the corrosion time is 15.3 h; the volume ratio of the sample liquid to the water is 0.57: 9;
(2) mixing acid liquor used in corrosion with water, detecting for 3 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of a sample by using S1 and S2; wherein the volume ratio of the acid liquid to the water is 1.17: 8.67.
The method realizes the detection of the grain size distribution and the size of the high-purity aluminum alloy sample, and the detection precision reaches 98 percent.
Example 6
The embodiment provides a method for testing the granularity of a high-purity aluminum alloy sample, which comprises the following steps:
(1) mixing a sample liquid obtained by corroding a high-purity aluminum alloy sample (not less than 3N) with water, detecting for 3 times by using a liquid particle counter, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water; shearing, pickling and drying the high-purity aluminum alloy sample in sequence before corrosion; the maximum length of the high-purity aluminum alloy sample after being sheared into pieces is 1.7 cm; the pickling time is 2.6 min; the washing liquid in the acid washing is a mixed liquid of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid, hydrofluoric acid and water in the mixed solution is 4.2:0.56: 0.98; the volume ratio of the hydrochloric acid to the water in the mixed solution is 0.65: 1; the corrosion time is 16.7 h; the volume ratio of the sample liquid to the water is 0.8: 9.1;
(2) mixing acid liquor used in corrosion with water, detecting for 3 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of a sample by using S1 and S2; wherein the volume ratio of the acid liquid to the water is 1.37: 9.23.
The method realizes the detection of the grain size distribution and the size of the high-purity aluminum alloy sample, and the detection precision reaches 98 percent.
Comparative example 1
The difference from example 1 is only that the acid washing time is 1min, sufficient detection conditions cannot be provided, and the detection accuracy is 30% lower.
Comparative example 2
The difference from the example 1 is only that the volume ratio of the nitric acid, the hydrofluoric acid and the water in the mixed solution is 12:1:1, the excessive addition of the nitric acid causes a violent reaction, sufficient detection conditions cannot be provided, and the accuracy is lower than 20%.
Comparative example 4
The difference from example 1 is only that the volume ratio of nitric acid, hydrofluoric acid and water in the mixed solution is 4:4:1, and the hydrofluoric acid is too much, so that the sample is processed too much, sufficient detection conditions cannot be provided, and the accuracy is lower by 35%.
Comparative example 5
The difference from example 1 is only that the volume ratio of nitric acid, hydrofluoric acid and water in the mixed solution is 4:1:4, and the addition amount of water is too large, which affects the pickling result, and sufficient detection conditions cannot be provided, so that the particle size distribution and size of the high-purity aluminum alloy sample cannot be detected.
Comparative example 6
The difference from the example 1 is only that the volume ratio of the hydrochloric acid to the water in the mixed solution is 0.3:1, the content of the hydrochloric acid in the mixed solution is low, the treatment degree is low, and the particle size distribution and the size of the high-purity aluminum alloy sample cannot be detected.
Comparative example 7
The difference from example 1 is only that the volume ratio of hydrochloric acid to water in the mixed solution is 2:1, resulting in excessive sample handling, failure to provide sufficient detection conditions, and a lower accuracy of 35%.
Comparative example 8
The difference from example 1 is only that the particle size distribution and size of the high purity aluminum alloy sample could not be detected by replacing the hydrochloric acid in the mixed solution with an equal amount of nitric acid.
According to the results of the embodiment and the comparative example, the testing method provided by the invention realizes the detection of the particle size distribution and the size of the high-purity aluminum alloy sample by using the liquid particle counter through the reasonable design of the testing steps, and meanwhile, the detection precision and the efficiency are also obviously improved, and the detection precision can reach more than 95%.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions 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 method for testing the granularity of the high-purity aluminum alloy sample is characterized by comprising the following steps of:
(1) mixing a sample liquid obtained after the high-purity aluminum alloy sample is corroded with water, detecting for at least 3 times by using a liquid particle counter, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water;
(2) mixing acid solution used in corrosion with water, detecting at least 3 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of the sample by using S1 and S2.
2. The test method according to claim 1, wherein the high purity aluminum alloy sample in step (1) is subjected to shearing, pickling and drying in sequence before corrosion.
3. The test method according to claim 2, wherein the high purity aluminum alloy sample has a maximum length of 1 to 3cm after shearing.
4. The test method according to claim 2 or 3, wherein the acid washing time is 2-5 min.
5. The test method according to any one of claims 2 to 4, wherein the washing liquid in the pickling is a mixed liquid of nitric acid, hydrofluoric acid and water.
6. The method of claim 5, wherein the volume ratio of the nitric acid, the hydrofluoric acid and the water in the mixed solution is (3-5): (0.5-1.5).
7. The test method according to any one of claims 1 to 6, wherein the volume ratio of hydrochloric acid to water in the mixed solution is (0.5-0.7): 1;
preferably, the etching time is 14-17 h.
8. The test method according to any one of claims 1 to 7, wherein the volume ratio of the sample liquid and water in step (1) is (0.5-1.5): (8.5-9.5).
9. The test method according to any one of claims 1 to 8, wherein the volume ratio of the acid solution to the water in the step (2) is (0.5-1.5): (8.5-9.5).
10. The test method of any one of claims 1-9, wherein the test method comprises:
(1) mixing a sample liquid obtained after the high-purity aluminum alloy sample is corroded with water, detecting for at least 3 times by using a liquid particle counter, and taking an average value S1; wherein the acid solution in the corrosion is a mixed solution of hydrochloric acid and water; shearing, pickling and drying the high-purity aluminum alloy sample in sequence before corrosion; the maximum length of the high-purity aluminum alloy sample after being cut into pieces is 1-3 cm; the pickling time is 2-5 min; the washing liquid in the acid washing is a mixed liquid of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid, hydrofluoric acid and water in the mixed solution is (3-5) to (0.5-1.5); the volume ratio of the hydrochloric acid to the water in the mixed solution is (0.5-0.7) to 1; the corrosion time is 14-17 h; the volume ratio of the sample liquid to the water is (0.5-1.5) to (8.5-9.5);
(2) mixing acid liquor used in corrosion with water, detecting for at least 3 times by using a liquid particle counter, taking an average value S2, and calculating the granularity of a sample by using S1 and S2; wherein the volume ratio of the acid liquid to the water is (0.5-1.5) to (8.5-9.5).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102374962A (en) * | 2010-08-26 | 2012-03-14 | 天津荣程联合钢铁集团有限公司 | Austenite grain size display method of wire rod for prestressed steel stranded wire |
| CN103344532A (en) * | 2013-06-19 | 2013-10-09 | 武汉理工大学 | Rapid metallographic determination method for grain size of GCr15 steel bearing assembly |
| CN103487309A (en) * | 2013-08-27 | 2014-01-01 | 中国船舶重工集团公司第七二五研究所 | Method for displaying grain size of metal material |
| CN104005078A (en) * | 2012-06-21 | 2014-08-27 | 诺发系统公司 | Electroplating apparatuses and methods employing liquid particle counter modules |
| CN106498399A (en) * | 2016-11-22 | 2017-03-15 | 河南平芝高压开关有限公司 | A kind of fine aluminium grain size caustic and preparation method thereof, corrodes process for show |
| CN111074279A (en) * | 2018-10-22 | 2020-04-28 | 宁波江丰电子材料股份有限公司 | Target corrosive agent and application method thereof |
| CN111198116A (en) * | 2018-11-20 | 2020-05-26 | 宁波江丰电子材料股份有限公司 | Target detection method |
| 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 |
-
2020
- 2020-07-13 CN CN202010668574.1A patent/CN111751254A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102374962A (en) * | 2010-08-26 | 2012-03-14 | 天津荣程联合钢铁集团有限公司 | Austenite grain size display method of wire rod for prestressed steel stranded wire |
| CN104005078A (en) * | 2012-06-21 | 2014-08-27 | 诺发系统公司 | Electroplating apparatuses and methods employing liquid particle counter modules |
| CN103344532A (en) * | 2013-06-19 | 2013-10-09 | 武汉理工大学 | Rapid metallographic determination method for grain size of GCr15 steel bearing assembly |
| CN103487309A (en) * | 2013-08-27 | 2014-01-01 | 中国船舶重工集团公司第七二五研究所 | Method for displaying grain size of metal material |
| CN106498399A (en) * | 2016-11-22 | 2017-03-15 | 河南平芝高压开关有限公司 | A kind of fine aluminium grain size caustic and preparation method thereof, corrodes process for show |
| CN111074279A (en) * | 2018-10-22 | 2020-04-28 | 宁波江丰电子材料股份有限公司 | Target corrosive agent and application method thereof |
| CN111198116A (en) * | 2018-11-20 | 2020-05-26 | 宁波江丰电子材料股份有限公司 | Target detection method |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 彭银仙 等, 哈尔滨工程大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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