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 PDF

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Publication number
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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CN106498399B (en
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马晓红
段冲
刘喜
孙明道
肖鹤旋
张田甜
王晓生
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Henan Pingzhi High Voltage Switchgear Co Ltd
State Grid Corp of China SGCC
Pinggao Group Co Ltd
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Henan Pingzhi High Voltage Switchgear Co Ltd
State Grid Corp of China SGCC
Pinggao Group 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
    • C23FNON-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
    • C23F1/00Etching metallic material by chemical means
    • C23F1/10Etching compositions
    • C23F1/14Aqueous compositions
    • C23F1/16Acidic compositions
    • C23F1/20Acidic compositions for etching aluminium or alloys thereof
    • 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
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02Investigating 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)
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  • 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

A kind of fine aluminium grain size caustic and preparation method thereof, corrodes process for show
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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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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CN103993319A (en) * 2014-05-06 2014-08-20 上海大学 Corrosive agent and display method for macrostructure of aluminum and aluminum copper alloys
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CN102103051A (en) * 2011-01-13 2011-06-22 马鞍山钢铁股份有限公司 Medium-high carbon steel actual grain size developer and developing method
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Cited By (6)

* Cited by examiner, † Cited by third party
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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