CN111501050A - Surface treatment method of ultra-high purity aluminum - Google Patents

Surface treatment method of ultra-high purity aluminum Download PDF

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Publication number
CN111501050A
CN111501050A CN202010368135.9A CN202010368135A CN111501050A CN 111501050 A CN111501050 A CN 111501050A CN 202010368135 A CN202010368135 A CN 202010368135A CN 111501050 A CN111501050 A CN 111501050A
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washing
acid
rinsing
purity aluminum
time
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姚力军
潘杰
边逸军
王学泽
任聪聪
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/12Light metals
    • C23G1/125Light metals aluminium
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • C23G5/02Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
    • C23G5/024Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing hydrocarbons
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • C23G5/02Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
    • C23G5/032Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/68Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using electric discharge to ionise a gas

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  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Mechanical Engineering (AREA)
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  • Organic Chemistry (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
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  • General Physics & Mathematics (AREA)
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  • Electrochemistry (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The invention relates to a surface treatment method of ultra-high purity aluminum, which comprises the following steps: and sequentially carrying out primary rinsing, acid washing, secondary rinsing and drying on the ultra-high purity aluminum. The method provided by the invention realizes the improvement of the detection accuracy of the glow discharge mass spectrum by reasonably designing each step in the processing method and utilizing the synergistic coupling effect among the steps, and simultaneously shortens the detection time to 25-50% of the detection time of the untreated high-purity aluminum.

Description

Surface treatment method of ultra-high purity aluminum
Technical Field
The invention relates to the field of surface treatment, in particular to a surface treatment method of ultra-high purity aluminum.
Background
Ultra-high purity aluminum, generally having a total purity of greater than 5N (> 99.999%), is mainly used for making sputtering targets. Before the method is used, a glow discharge mass spectrometer is generally used for detecting the content of trace elements in materials, and Glow Discharge Mass Spectrometry (GDMS) is the most effective method for analyzing trace impurity components of trace solid conductive materials at present. Glow discharge mass spectrometry has the advantages of high sensitivity, low detection limit, wide element analysis range and the like. The glow discharge mass spectrum consists of a glow discharge ion source and a mass spectrometer. The glow discharge ion source utilizes inert gas (generally argon) to generate ions ionized under the voltage of thousands of volts to impact the surface of a sample to generate sputtering (namely atomization), the sputtered atoms are diffused into plasma to be further ionized, and are respectively focused in direction and energy through a magnetic field and an electric field, and then are collected and detected by a detector.
Currently, the most internationally used glow discharge mass spectra include Nu Astrum, VG9000, Element GD and the like. NuAstrum and VG9000 use tantalum material in large quantities in sample cells, ion sources, sample holders. Tantalum, when present in a plasma, tends to combine with gases such as carbon, hydrogen, oxygen, nitrogen, etc., thereby effectively eliminating interference from residual gases, making the mass spectrum simple and easy to analyze. In the routine test process, the tantalum part in the GDMS is gradually polluted due to deposition of sample atoms, and needs to be replaced and cleaned according to a certain frequency. For example, CN108212912A discloses a method for cleaning a ceramic wafer for glow discharge mass spectrometry, which comprises: providing a ceramic wafer for glow discharge mass spectrometry equipment; carrying out a first cleaning process on the ceramic wafer; after the first cleaning process, performing a second cleaning process on the ceramic wafer, wherein the second cleaning process comprises an ultrasonic cleaning process; and after the second cleaning process, drying the ceramic wafer at a preset temperature. The first cleaning process is mainly used for removing metal impurities on the surface of the ceramic wafer, and the ceramic wafer is provided with a plurality of micropores, so that impurities (such as metal dissolved matters after the first cleaning process) are easily adsorbed in the micropores, residual impurities in the micropores after the first cleaning process can be effectively removed through the ultrasonic cleaning process, and residual impurities with low melting point in the micropores can be evaporated when the drying process is carried out at a preset temperature, so that the impurity removal effect on the ceramic wafer is improved, the impurity residues of the ceramic wafer are reduced, and the detection accuracy and the detection efficiency of the glow discharge mass spectrum are improved.
However, impurities exist on the surface of the high-purity aluminum sample, which leads to inaccurate detection results.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a surface treatment method of ultra-high purity aluminum, which can remarkably improve the detection accuracy of glow discharge mass spectrometry and remarkably shorten the detection time.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a surface treatment method of ultra-high purity aluminum, which comprises the following steps: and sequentially carrying out primary rinsing, acid washing, secondary rinsing and drying on the ultra-high purity aluminum.
The method provided by the invention realizes the improvement of the detection accuracy of the glow discharge mass spectrum by reasonably designing each step in the processing method and utilizing the synergistic coupling effect among the steps, and simultaneously shortens the detection time to 25-50% of the detection time of the untreated high-purity aluminum.
As a preferred embodiment of the present invention, the washing solution of the first rinsing includes 1 or a combination of at least 2 of toluene, xylene, acetone, or ethanol.
In a preferred embodiment of the present invention, the first rinsing time is 2 to 4min, for example, 2min, 2.2min, 2.4min, 2.6min, 2.8min, 3min, 3.2min, 3.4min, 3.6min, 3.8min, or 4min, 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 cleaning solution in the acid cleaning is a mixed acid solution of nitric acid, hydrofluoric acid, and water.
Preferably, the volume ratio of nitric acid, hydrofluoric acid and water in the mixed acid solution is (0.5-1.5): (0.5-1.5): (3.5-4.5), and may be, for example, 0.5:0.5:3.5, 1:0.5:3.5, 1.5:0.5:3.5, 0.5:1:3.5, 0.5:1.5:3.5, 0.5:0.5:4, 0.5:0.5:4.5, 1:1:3.5, 1:1:4 or 1:1:4.5, but not limited to the recited values, and other values not recited in this range are equally applicable.
In a preferred embodiment of the present invention, the acid washing time is 10 to 20 seconds, and may be, for example, 10 seconds, 11 seconds, 12 seconds, 13 seconds, 14 seconds, 15 seconds, 16 seconds, 17 seconds, 18 seconds, 19 seconds, or 20 seconds, 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 is performed at least 2 times, for example, 2 times, 3 times, 4 times, 5 times, 6 times, 7 times, or 8 times, but the present invention is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
As a preferred embodiment of the present invention, the second rinsing includes water washing and ethanol washing performed in this order.
In a preferred embodiment of the present invention, the washing time is 2 to 4 seconds, and may be, for example, 2s, 2.2s, 2.4s, 2.6s, 2.8s, 3s, 3.2s, 3.4s, 3.6s, 3.8s, or 4s, but is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
Preferably, the water washing is performed 2 to 3 times.
In a preferred embodiment of the present invention, the time for the ethanol washing is 2 to 4 seconds, and may be, for example, 2s, 2.2s, 2.4s, 2.6s, 2.8s, 3s, 3.2s, 3.4s, 3.6s, 3.8s, or 4s, but is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
Preferably, the number of ethanol washes is 2-3.
As a preferred technical solution of the present invention, the method comprises: sequentially carrying out first rinsing, acid washing, second rinsing and drying on the ultra-high purity aluminum; the first rinse wash comprises 1 or a combination of at least 2 of toluene, xylene, acetone, or ethanol; the first rinsing time is 2-4 min; the washing liquid in the acid washing is a mixed acid solution of nitric acid, hydrofluoric acid and water; the volume ratio of the nitric acid to the hydrofluoric acid to the water in the mixed acid solution is (0.5-1.5) to (3.5-4.5); the pickling time is 10-20 s; the acid washing is carried out for at least 4 times; the second rinsing comprises water washing and ethanol washing which are sequentially carried out; the washing time is 2-4 s; the water washing is carried out for 2-3 times; the ethanol cleaning time is 2-4 s; the number of times of ethanol cleaning is 2-3.
Compared with the prior art, the invention at least has the following beneficial effects:
the method provided by the invention realizes the improvement of the detection accuracy of the glow discharge mass spectrum by reasonably designing each step in the processing method and utilizing the synergistic coupling effect among the steps, and simultaneously shortens the detection time to 25-50% of the detection time of the untreated high-purity aluminum.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
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 invention provides a surface treatment method of ultra-high purity aluminum, which comprises the following steps: sequentially carrying out first rinsing, acid washing, second rinsing and drying on the ultra-high purity aluminum; the washing liquid of the first rinsing comprises acetone; the time of the first rinsing is 3 min; the washing liquid in the acid washing is a mixed acid solution of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid, hydrofluoric acid and water in the mixed acid solution is 0.5:1.1: 4; the pickling time is 16 s; the acid washing is carried out for 5 times; the second rinsing comprises water washing and ethanol washing which are sequentially carried out; the washing time is 3 s; the water washing is carried out for 2 times; the ethanol cleaning time is 2 s; the number of times of ethanol washing is 2.
After the ultrahigh-purity aluminum is treated, the detection accuracy of the glow discharge mass spectrum is improved, and the detection time is shortened to 30% of that of untreated high-purity aluminum.
Example 2
The invention provides a surface treatment method of ultra-high purity aluminum, which comprises the following steps: sequentially carrying out first rinsing, acid washing, second rinsing and drying on the ultra-high purity aluminum; the first rinse wash comprises ethanol; the time of the first rinsing is 4 min; the washing liquid in the acid washing is a mixed acid solution of nitric acid, hydrofluoric acid and water; the volume ratio of the nitric acid to the hydrofluoric acid to the water in the mixed acid solution is 1.5:1.5: 3.5; the pickling time is 12 s; the acid washing is carried out for 2 times; the second rinsing comprises water washing and ethanol washing which are sequentially carried out; the washing time is 2 s; the water washing is carried out for 3 times; the ethanol cleaning time is 4 s; the number of times of ethanol washing is 2.
After the ultrahigh-purity aluminum is treated, the detection accuracy of the glow discharge mass spectrum is improved, and the detection time is shortened to 45% of that of untreated high-purity aluminum.
Example 3
The invention provides a surface treatment method of ultra-high purity aluminum, which comprises the following steps: sequentially carrying out first rinsing, acid washing, second rinsing and drying on the ultra-high purity aluminum; the wash liquor of the first rinse comprises toluene; the time of the first rinsing is 2 min; the washing liquid in the acid washing is a mixed acid solution of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid to hydrofluoric acid to water in the mixed acid solution is 0.7:1: 3.7; the pickling time is 12 s; the acid washing is carried out for 7 times; the second rinsing comprises water washing and ethanol washing which are sequentially carried out; the washing time is 2 s; the water washing is carried out for 2 times; the ethanol cleaning time is 2 s; the number of times of ethanol washing is 2.
After the ultrahigh-purity aluminum is treated, the detection accuracy of the glow discharge mass spectrum is improved, and the detection time is shortened to 25% of that of untreated high-purity aluminum.
Example 4
The invention provides a surface treatment method of ultra-high purity aluminum, which comprises the following steps: sequentially carrying out first rinsing, acid washing, second rinsing and drying on the ultra-high purity aluminum; the washing liquid of the first rinsing comprises acetone; the time of the first rinsing is 4 min; the washing liquid in the acid washing is a mixed acid solution of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid to hydrofluoric acid to water in the mixed acid solution is 0.8:0.5: 4.2; the pickling time is 17 s; the acid washing is carried out for 4 times; the second rinsing comprises water washing and ethanol washing which are sequentially carried out; the washing time is 2 s; the water washing is carried out for 2 times; the ethanol cleaning time is 2 s; the number of times of ethanol washing is 2.
After the ultrahigh-purity aluminum is treated, the detection accuracy of the glow discharge mass spectrum is improved, and the detection time is shortened to 45% of that of untreated high-purity aluminum.
Example 5
The invention provides a surface treatment method of ultra-high purity aluminum, which comprises the following steps: sequentially carrying out first rinsing, acid washing, second rinsing and drying on the ultra-high purity aluminum; the wash liquor of the first rinse comprises xylene; the time of the first rinsing is 4 min; the washing liquid in the acid washing is a mixed acid solution of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid to hydrofluoric acid to water in the mixed acid solution is 1.2:0.7: 3.5; the pickling time is 12 s; the acid washing is carried out for 6 times; the second rinsing comprises water washing and ethanol washing which are sequentially carried out; the washing time is 4 s; the water washing is carried out for 3 times; the ethanol cleaning time is 3 s; the number of times of ethanol washing is 2.
After the ultrahigh-purity aluminum is treated, the detection accuracy of the glow discharge mass spectrum is improved, and the detection time is shortened to 35% of that of untreated high-purity aluminum.
Example 6
The invention provides a surface treatment method of ultra-high purity aluminum, which comprises the following steps: sequentially carrying out first rinsing, acid washing, second rinsing and drying on the ultra-high purity aluminum; the washing liquid of the first rinsing is ethanol; the time of the first rinsing is 3.7 min; the washing liquid in the acid washing is a mixed acid solution of nitric acid, hydrofluoric acid and water; the volume ratio of nitric acid, hydrofluoric acid and water in the mixed acid solution is 1:0.75: 4; the pickling time is 13 s; the acid washing is carried out for 3 times; the second rinsing comprises water washing and ethanol washing which are sequentially carried out; the washing time is 3 s; the water washing is carried out for 3 times; the ethanol cleaning time is 3 s; the number of times of ethanol washing is 3.
After the ultrahigh-purity aluminum is treated, the detection accuracy of the glow discharge mass spectrum is improved, and the detection time is shortened to 47% of that of untreated high-purity aluminum.
Comparative example 1
The difference from the example 1 is only that the volume ratio of the nitric acid to the hydrofluoric acid to the water in the mixed acid solution is 0.1:1.1:4, the detection accuracy of the glow discharge mass spectrum is not improved after the ultra-high purity aluminum treatment, and the detection time is not shortened.
Comparative example 2
The difference from the example 1 is only that the volume ratio of the nitric acid to the hydrofluoric acid to the water in the mixed acid solution is 2:1.1:4, the detection accuracy of the glow discharge mass spectrum is not improved and the detection time is not shortened after the ultra-high purity aluminum treatment.
Comparative example 3
The difference from the example 1 is only that the volume ratio of the nitric acid to the hydrofluoric acid to the water in the mixed acid solution is 0.5:0.1:4, the detection accuracy of the glow discharge mass spectrum is not improved after the ultra-high purity aluminum treatment, and the detection time is not shortened.
Comparative example 4
The difference from the example 1 is only that the volume ratio of the nitric acid to the hydrofluoric acid to the water in the mixed acid solution is 0.5:3:4, the detection accuracy of the glow discharge mass spectrum is not improved and the detection time is not shortened after the ultra-high purity aluminum treatment.
Comparative example 5
The difference from the example 1 is only that the volume ratio of the nitric acid to the hydrofluoric acid to the water in the mixed acid solution is 0.5:1.1:2, the detection accuracy of the glow discharge mass spectrum is not improved after the ultra-high purity aluminum treatment, and the detection time is not shortened.
Comparative example 6
The difference from the example 1 is only that the volume ratio of the nitric acid to the hydrofluoric acid to the water in the mixed acid solution is 0.5:1.1:6, the detection accuracy of the glow discharge mass spectrum is not improved after the ultra-high purity aluminum treatment, and the detection time is not shortened.
Comparative example 7
The difference from example 1 is only that the first rinsing is not performed, and the detection accuracy of the glow discharge mass spectrum is not improved and the detection time is not shortened after the ultra-high purity aluminum treatment.
Comparative example 8
The difference from example 1 is only that no acid washing is performed, and the detection accuracy of the glow discharge mass spectrum is not improved and the detection time is not shortened after the ultra-high purity aluminum treatment.
Comparative example 9
The difference from example 1 is only that the second rinsing is not performed, and the detection accuracy of the glow discharge mass spectrum is not improved and the detection time is not shortened after the ultra-high purity aluminum treatment.
Comparative example 10
The difference from example 1 is only that the order of the first rinsing and the acid washing is changed, and the detection accuracy of the glow discharge mass spectrum is not improved and the detection time is not shortened after the ultra-high purity aluminum treatment.
Comparative example 11
The difference from example 1 is only that the order of the second rinsing and the acid washing is changed, and the detection accuracy of the glow discharge mass spectrum is not improved and the detection time is not shortened after the ultra-high purity aluminum treatment.
Comparative example 12
The difference from the example 1 is only that the order of the first rinsing and the second rinsing is changed, and the detection accuracy of the glow discharge mass spectrum is not improved and the detection time is not shortened after the ultra-high purity aluminum treatment.
Comparative example 13
The difference from the example 1 is only that the acid washing time is 10s, the detection accuracy of the glow discharge mass spectrum is not improved and the detection time is not shortened after the ultra-high purity aluminum treatment.
Comparative example 14
The difference from the example 1 is only that the acid washing time is 50s, the detection accuracy of the glow discharge mass spectrum is not improved and the detection time is not shortened after the ultra-high purity aluminum treatment.
According to the results of the embodiment and the comparative example, the method provided by the invention realizes the improvement of the detection accuracy of the glow discharge mass spectrum by reasonably designing the steps in the treatment method and utilizing the synergistic coupling effect among the steps, and simultaneously shortens the detection time to 25-50% of the detection time of the untreated high-purity aluminum.
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. A surface treatment method of ultra-high purity aluminum, characterized by comprising: and sequentially carrying out primary rinsing, acid washing, secondary rinsing and drying on the ultra-high purity aluminum.
2. The method of claim 1, wherein the first rinse wash solution comprises 1 or a combination of at least 2 of toluene, xylene, acetone, or ethanol.
3. The method of claim 1 or 2, wherein the first rinsing time is 2-4 min.
4. The method according to any one of claims 1 to 3, wherein the washing liquid in the acid washing is a mixed acid solution of nitric acid, hydrofluoric acid and water;
preferably, the volume ratio of the nitric acid to the hydrofluoric acid to the water in the mixed acid solution is (0.5-1.5): (3.5-4.5).
5. The method of any one of claims 1-4, wherein the acid wash time is 10-20 s.
6. The method of any one of claims 1-5, wherein the acid wash is performed at least 2 times.
7. The method of any of claims 1-6, wherein the second rinse comprises a water wash and an ethanol wash performed sequentially.
8. The method of claim 7, wherein the time of the water wash is 2-4 s;
preferably, the water washing is performed 2 to 3 times.
9. The method of claim 7 or 8, wherein the ethanol wash time is 2-4 s;
preferably, the number of ethanol washes is 2-3.
10. The method of any one of claims 1-9, wherein the method comprises: sequentially carrying out first rinsing, acid washing, second rinsing and drying on the ultra-high purity aluminum; the first rinse wash comprises 1 or a combination of at least 2 of toluene, xylene, acetone, or ethanol; the first rinsing time is 2-4 min; the washing liquid in the acid washing is a mixed acid solution of nitric acid, hydrofluoric acid and water; the volume ratio of the nitric acid to the hydrofluoric acid to the water in the mixed acid solution is (0.5-1.5) to (3.5-4.5); the pickling time is 10-20 s; the acid washing is carried out for at least 2 times; the second rinsing comprises water washing and ethanol washing which are sequentially carried out; the washing time is 2-4 s; the water washing is carried out for 2-3 times; the ethanol cleaning time is 2-4 s; the number of times of ethanol cleaning is 2-3.
CN202010368135.9A 2020-04-30 2020-04-30 Surface treatment method of ultra-high purity aluminum Pending CN111501050A (en)

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CN112345482A (en) * 2020-10-23 2021-02-09 宁波江丰电子材料股份有限公司 Analysis method for carbon content in aluminum material
CN113174487A (en) * 2021-04-13 2021-07-27 新疆众和股份有限公司 Recovery method of aluminum residual target for liquid crystal panel
CN113504291A (en) * 2021-06-16 2021-10-15 宁波锦越新材料有限公司 Sample preparation method and detection method for determining impurities in ultra-high-purity aluminum by utilizing ICP-MS (inductively coupled plasma-mass spectrometry)
CN113702485A (en) * 2021-09-17 2021-11-26 广东先导稀材股份有限公司 Method for measuring content of trace impurity elements in massive aluminum nitride
CN115505934A (en) * 2022-10-21 2022-12-23 同创普润(上海)机电高科技有限公司 Pretreatment method for remelting and utilizing ultra-pure aluminum ingot for semiconductor

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