CN106498399A - A kind of fine aluminium grain size caustic and preparation method thereof, corrodes process for show - Google Patents
A kind of fine aluminium grain size caustic and preparation method thereof, corrodes process for show Download PDFInfo
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- CN106498399A CN106498399A CN201611046194.4A CN201611046194A CN106498399A CN 106498399 A CN106498399 A CN 106498399A CN 201611046194 A CN201611046194 A CN 201611046194A CN 106498399 A CN106498399 A CN 106498399A
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- caustic
- fine aluminium
- acid
- polishing
- grain size
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 49
- 239000004411 aluminium Substances 0.000 title claims abstract description 46
- 239000003518 caustics Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 19
- 238000005260 corrosion Methods 0.000 claims abstract description 18
- 230000007797 corrosion Effects 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 16
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 7
- 238000005498 polishing Methods 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 13
- 238000005516 engineering process Methods 0.000 claims description 4
- 230000003628 erosive effect Effects 0.000 claims description 4
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000007517 polishing process Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 239000004576 sand Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 11
- 238000013329 compounding Methods 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- XMXNVYPJWBTAHN-UHFFFAOYSA-N potassium chromate Chemical compound [K+].[K+].[O-][Cr]([O-])(=O)=O XMXNVYPJWBTAHN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/20—Acidic compositions for etching aluminium or alloys thereof
-
- 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
- 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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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- ing And Chemical Polishing (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The present invention relates to a kind of fine aluminium grain size caustic and preparation method thereof, corrodes process for show.The fine aluminium grain size caustic is composed of the following components:K2CrO45~7g, 6~10ml of nitric acid, picric acid saturated aqueous solution 1ml, 0.4~0.6ml of Fluohydric acid., 4~8ml of hydrochloric acid, 18~22ml of water.Pure aluminum substrate is single αsolidsolution, and αsolidsolution has different position phases, produces crystal boundary after corrosion, existing caustic and caustic solution implement after fine aluminium crystal boundary is more difficult obvious level difference, corrosive effect is poor.The fine aluminium grain size caustic of the present invention, is formed by nitric acid, Fluohydric acid., hydrochloric acid, Neutral potassium chromate, picric acid compounding, K2CrO4Concentration suitable, the effect of oxidant and mordant can be simultaneously worked as, the α crystal grain of different position phases can be dyeed while crystal boundary is corroded, coordinate picric effect to make crystal boundary more prominent, clear.
Description
Technical field
The invention belongs to pure aluminum material physical and chemical inspection technical field, and in particular to a kind of fine aluminium grain size caustic and its system
Preparation Method, corrodes process for show.
Background technology
In High-Voltage Electrical Appliances engineering insulating mechanism, electric field is uneven mostly, if internal field is very strong, less high
Under voltage, shelf depreciation just occurs, or even occur puncturing, it is therefore desirable to take measures to improve Electric Field Distribution, reduce local mistake
High field intensity, the overall dielectric intensity of raising insulation system, and radome used in insulating mechanism, shielding part, grading ring etc.
The part of special construction is to improve the maximally effective measure of this phenomenon.
The splendid forming characteristic of fine aluminium, highly corrosion resistant, good weldability and electric conductivity can bear various pressure
Process and extend, bend so as to become processing radome, shielding part, the optimal material of grading ring part.But radome etc. is holding
Mechanical load, electric power or mechanical vibration being also subject to while receiving electric field, and fine aluminium being not heat-treatable strengthened material, which is organized
The quality of state it is critical only that size, form and the distribution of grain size, so understanding the size of crystal grain, form and distribution tool in time
Significant.Be analyzed for the performance needed for obtaining and to material property change mechanism, need crystal grain to be carried out to material
Degree analysis.
But the grain size state of fine aluminium to be observed, the particularly fine aluminium of annealed state, it is difficult to crystal boundary is clearly visible that,《Metal
Material fractograph》The NaOH aqueous corrosion agent provided in one book, requires heat to 50~70 DEG C, and easily in the table of sample
Face forms one layer of film like pollution layer for being difficult to remove, and causes observation fuzzy, and crystal boundary is difficult to recognize at all.
GB/T3246.1-2012《Deformation aluminum and Al-alloy products histological test method》No. 2 fine aluminium grain boundary corrosions for providing
Agent completely cannot show crystal boundary to the fabricated product of annealed state, can only be observed by anode masking biasing light, but this sight
Examine method not only to take, and improve cost of manufacture, so one kind is urgently needed when checking fine aluminium grain size conveniently
Caustic and efficient easily corrosion process for show.
Content of the invention
It is an object of the invention to provide a kind of applicable High-Voltage Electrical Appliances industry fine aluminium grain size caustic, existing so as to solve
The corrosive effect of caustic is bad or operation not easily problem.
Second object of the present invention is to provide the preparation method of above-mentioned fine aluminium grain size caustic.
Third object of the present invention is to provide a kind of corrosion process for show.
In order to realize that object above, the technical solution adopted in the present invention be:
A kind of fine aluminium grain size caustic, composed of the following components:K2CrO45~7g, 6~10ml of nitric acid, picric acid satisfy
With aqueous solution 1ml, 0.4~0.6ml of Fluohydric acid., 4~8ml of hydrochloric acid, 18~22ml of water;The mass concentration of the nitric acid be 65%~
68%, the mass concentration of Fluohydric acid. is at least 40%, and the mass concentration of hydrochloric acid is 36%~38%.Above component value can by than
Example is zoomed in or out.
Preferably, above-mentioned fine aluminium grain size caustic, composed of the following components:K2CrO46g, nitric acid 8ml, picric acid satisfy
With aqueous solution 1ml, Fluohydric acid. 0.5ml, hydrochloric acid 6ml, water 20.5ml.
Pure aluminum substrate is single αsolidsolution, and αsolidsolution has different position phases, produces crystal boundary after corrosion, but due to not
Difference with the electrode potential of the α phase crystal grain of position phase is less and corrosion-resistant, and after existing caustic and caustic solution enforcement, fine aluminium is brilliant
Boundary is more difficult obvious level difference, and corrosive effect is poor.The fine aluminium grain size caustic that the present invention is provided, by nitric acid, hydrogen fluorine
Acid, hydrochloric acid, Neutral potassium chromate, picric acid compounding are formed, K2CrO4Concentration suitable, the effect of oxidant and mordant can be simultaneously worked as,
The α crystal grain of different position phases can be dyeed while crystal boundary is corroded, coordinate picric effect to make crystal boundary more prominent, clear.
The preparation method of above-mentioned fine aluminium grain size caustic, comprises the following steps:
1) mixing of 0.4~0.6ml Fluohydric acid .s, 4~8ml hydrochloric acid, 3~5ml nitric acid and 0.5ml water is taken, solution A is made;To 5
~7g K2CrO4Middle addition 3~5ml nitric acid is dissolved, then is mixed with 17.5~21.5ml water, 1ml picric acid saturated aqueous solutions
Close, obtain solution B;
2) solution A and solution B are mixed, is obtained final product.
The preparation method of the fine aluminium grain size caustic that the present invention is provided, process is simple, safety are good, it is easy to operate, and fit
Close industrialized production application.
A kind of corrosion process for show using above-mentioned fine aluminium grain size caustic, comprises the following steps:
1) prepared by sample:By polishing, polishing after cold for fine aluminium sample inlaying, polishing sample is made;
2) dust technology cleaning polishing specimen surface is used, then is rinsed with water, dried;
3) using fine aluminium grain size caustic wipe erosion step 2) process after polishing 5~15s of sample, cleaned with water and done
Dry, you can be observed.
Step 1) in, the polishing is to adopt 400#, 600#, 800#, 1200#, 2500#, 4000# diamond sand paper successively
Polishing fine aluminium sample.
Step 1) in, the polishing fluid used by the polishing is by the NaOH solution that alumina polishing solution and mass concentration are 5%
Mix, alumina polishing solution is 10 with the volume ratio of NaOH solution:1.Preferably can be eliminated using the polishing fluid tiny
Cut.In alumina polishing solution, the particle diameter of aluminium oxide is 0.05~0.3 μm.Preferably, in polishing process, the rotating speed of polished machine is
100~300r/min, the pressure of applying is 15~20N.
The corrosion process for show that the present invention is provided, easy to operate, without the need for heating, favorable reproducibility, it is not necessary to electrolytic anode system
Film, low cost, high working efficiency.
Description of the drawings
Fig. 1 is corrosion corrosive effect figure of the process for show to annealed state fine aluminium sample using the embodiment of the present invention 1
(50X).
Specific embodiment
With reference to specific embodiment, the invention will be further described.In following examples, the mass concentration of hydrochloric acid is
36%~38%, the mass concentration of nitric acid is 65%~68%, and the mass concentration of Fluohydric acid. is 40%, picric acid saturated aqueous solution
Mass concentration be 1.2%, agents useful for same is the pure level of commercially available analysis.
Embodiment 1
The fine aluminium grain size caustic of the present embodiment, composed of the following components:K2CrO46g, nitric acid 8ml, picric acid saturation
Aqueous solution 1ml, Fluohydric acid. 0.5ml, hydrochloric acid 6ml, water 20.5ml.
The preparation method of the fine aluminium grain size caustic of the present embodiment, comprises the following steps:
1) Fluohydric acid. of 0.5ml, the hydrochloric acid of 6ml, the nitric acid of 3ml, the distilled water of 0.5ml are measured to be placed in beaker, is stirred
30s, makes solution A;Weigh 6g K2CrO4It is put in plastic beaker, measures 5ml nitric acid and pour in plastic beaker, stirs to molten
Solution, adds 1ml picric acid saturated aqueous solutions and 20ml distilled water mix homogeneously, obtains solution B;
2) solution A is mixed homogeneously with solution B, obtains final product.
The corrosion process for show of the present embodiment, comprises the following steps:
1) cut 20*20mm fine aluminium sample, cold inlay after using automatic grinding and polishing machine successively with 400#, 600#, 800#,
1200#, 2500#, 4000# diamond sand paper carries out water mill, then is polished with polishing fluid, makes polishing sample;Polishing fluid by
Mass ratio is 10:The NaOH solution composition of 1 alumina polishing solution and 5wt%, during grinding and polishing, the rotating speed of polished machine is 200r/
Min, the pressure of applying is 15N;
2) by step 1) (nitric acid is 1 with the volume ratio of distilled water to gained polishing sample dust technology:5) surface is cleaned, then
Rinsed well with water, then cleaned with alcohol swab and dried up;
3) using the method for wiping erosion, with the fine aluminium grain size caustic of the present embodiment by step 2) process after polishing sample
Erosion 10s is wiped, with the cold water flush for flowing and is dried up, you can observed.
After being processed through the present embodiment corrosion process for show, the corrosive effect figure of annealed state fine aluminium sample as shown in figure 1,
As seen from the figure, the crystal boundary of fine aluminium sample project, clear, disclosure satisfy that the Grain size analysis requirement of fine aluminium.
Embodiment 2
The fine aluminium grain size caustic of the present embodiment, composed of the following components:K2CrO45g, nitric acid 10ml, picric acid satisfy
With aqueous solution 1ml, Fluohydric acid. 0.4ml, hydrochloric acid 8ml, water 22ml.
The preparation method of the fine aluminium grain size caustic of the present embodiment, preparation method is with embodiment 1.
Embodiment 3
The fine aluminium grain size caustic of the present embodiment, composed of the following components:K2CrO47g, nitric acid 6ml, picric acid saturation
Aqueous solution 1ml, Fluohydric acid. 0.6ml, hydrochloric acid 4ml, water 18ml.
The preparation method of the fine aluminium grain size caustic of the present embodiment, preparation method is with embodiment 1.
Using the fine aluminium grain size caustic of embodiment 2 and embodiment 3, corrode the side of manifesting using 1 identical of same embodiment
Method is processed to fine aluminium sample, can obtain the suitable corrosive effect figure of effect.
Claims (8)
1. a kind of fine aluminium grain size caustic, it is characterised in that composed of the following components:K2CrO45~7g, 6~10ml of nitric acid,
Picric acid saturated aqueous solution 1ml, 0.4~0.6ml of Fluohydric acid., 4~8ml of hydrochloric acid, 18~22ml of water;The mass concentration of the nitric acid
For 65%~68%, the mass concentration of Fluohydric acid. is at least 40%, and the mass concentration of hydrochloric acid is 36%~38%.
2. fine aluminium grain size caustic as claimed in claim 1, it is characterised in that composed of the following components:K2CrO46g, nitre
Sour 8ml, picric acid saturated aqueous solution 1ml, Fluohydric acid. 0.5ml, hydrochloric acid 6ml, water 20.5ml.
3. a kind of preparation method of fine aluminium grain size caustic as claimed in claim 1, it is characterised in that including following step
Suddenly:
1) mixing of 0.4~0.6ml Fluohydric acid .s, 4~8ml hydrochloric acid, 3~5ml nitric acid and 0.5ml water is taken, solution A is made;To 5~7g
K2CrO4Middle addition 3~5ml nitric acid is dissolved, then is mixed with 17.5~21.5ml water, 1ml picric acid saturated aqueous solutions, is obtained
Solution B;
2) solution A and solution B are mixed, is obtained final product.
4. a kind of corrosion process for show using fine aluminium grain size caustic as claimed in claim 1 or 2, it is characterised in that
Comprise the following steps:
1) prepared by sample:By polishing, polishing after cold for fine aluminium sample inlaying, polishing sample is made;
2) dust technology cleaning polishing specimen surface is used, then is rinsed with water, dried;
3) using fine aluminium grain size caustic wipe erosion step 2) process after polishing 5~15s of sample, cleaned with water and dried, i.e.,
Can be observed.
5. corrosion process for show as claimed in claim 4, it is characterised in that step 1) in, the polishing is to adopt successively
400#, 600#, 800#, 1200#, 2500#, 4000# diamond sand papering fine aluminium sample.
6. the corrosion process for show as described in claim 4 or 5, it is characterised in that step 1) in, polishing used by the polishing
Liquid is mixed by the NaOH solution that alumina polishing solution and mass concentration are 5%, the body of alumina polishing solution and NaOH solution
Product is than being 10:1.
7. corrosion process for show as claimed in claim 6, it is characterised in that the particle diameter of aluminium oxide is in alumina polishing solution
0.05~0.3 μm.
8. the corrosion process for show as described in claim 4 or 5, it is characterised in that step 1) in, in polishing process, polished machine
Rotating speed be 100~300r/min of rotating speed, the pressure of applying is 15~20N.
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Cited By (6)
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CN107937975A (en) * | 2017-12-01 | 2018-04-20 | 佛山市高明高盛铝业有限公司 | A kind of wrought aluminium alloy preparation method of metallographic sample |
CN108893772A (en) * | 2018-05-14 | 2018-11-27 | 西安理工大学 | It is a kind of for showing the corrosive agent and caustic solution of almag metallographic structure |
CN111537320A (en) * | 2020-05-15 | 2020-08-14 | 宁波锦越新材料有限公司 | Sample preparation method for GDMS detection and sample |
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 |
CN112553628A (en) * | 2020-11-30 | 2021-03-26 | 晟通科技集团有限公司 | Aluminum alloy etching agent and aluminum alloy etching method |
CN115595582A (en) * | 2022-11-10 | 2023-01-13 | 中铁检验认证(常州)机车车辆配件检验站有限公司(Cn) | Aluminum alloy grain size etchant and application thereof |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107937975A (en) * | 2017-12-01 | 2018-04-20 | 佛山市高明高盛铝业有限公司 | A kind of wrought aluminium alloy preparation method of metallographic sample |
CN108893772A (en) * | 2018-05-14 | 2018-11-27 | 西安理工大学 | It is a kind of for showing the corrosive agent and caustic solution of almag metallographic structure |
CN111537320A (en) * | 2020-05-15 | 2020-08-14 | 宁波锦越新材料有限公司 | Sample preparation method for GDMS detection and sample |
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 |
CN112553628A (en) * | 2020-11-30 | 2021-03-26 | 晟通科技集团有限公司 | Aluminum alloy etching agent and aluminum alloy etching method |
CN115595582A (en) * | 2022-11-10 | 2023-01-13 | 中铁检验认证(常州)机车车辆配件检验站有限公司(Cn) | Aluminum alloy grain size etchant and application thereof |
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