CN106086906B - It is a kind of for clearing up the cleaning agent of steel macrostructure hot acid corrosion product - Google Patents

It is a kind of for clearing up the cleaning agent of steel macrostructure hot acid corrosion product Download PDF

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Publication number
CN106086906B
CN106086906B CN201610400889.1A CN201610400889A CN106086906B CN 106086906 B CN106086906 B CN 106086906B CN 201610400889 A CN201610400889 A CN 201610400889A CN 106086906 B CN106086906 B CN 106086906B
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China
Prior art keywords
cleaning agent
acid
cleaning
corrosion product
nitric acid
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Expired - Fee Related
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CN201610400889.1A
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CN106086906A (en
Inventor
王明建
夏申琳
潘恒沛
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725th Research Institute of CSIC
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725th Research Institute of CSIC
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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
    • C23G1/08Iron or steel
    • C23G1/085Iron or steel solutions containing HNO3
    • 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

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

Abstract

It is a kind of for clearing up the cleaning agent of steel macrostructure hot acid corrosion product, raw material is made of water, hydrochloric acid, nitric acid and neopelex, the present invention is by hydrochloric acid, nitric acid to the solvability of corrosion product, stronger cleaning gene is formed with neopelex to combine, and solves the problems, such as that cleaning effect is bad.

Description

It is a kind of for clearing up the cleaning agent of steel macrostructure hot acid corrosion product
Technical field
The invention belongs to a kind of metallographics of steel to detect cleaning technique, be mainly used for washed samples table when the detection of steel macrostructure The hot acid corrosion product in face, and the corrosion product for the steel that can not can be effectively cleared up existing cleaning agent is cleared up, and is reached Macrostructure specimen surface is neatly without the purpose of dirt.
Background technique
The method of existing cleaning steel macrostructure corrosion product are as follows: after macrostructure sample hot acid etches, take out With 3% ~ 5%(volumetric ratio) aqueous sodium carbonate or 10% ~ 15%(volumetric ratio) aqueous solution of nitric acid brushed, and is rinsed with clear water dry Only, it is finally dried up with dry air.
Ordinary steel material can effectively clear up corrosion product with the cleaning agent prepared above, but for Certain materials, such as 05Cr17Ni4Cu4Nb, GS-80, the cleaning effect of existing cleaning agent will but have a greatly reduced quality, and give macrostructure Detection grading brings very big puzzlement, sees Fig. 1.By inquiring domestic and international related data, significantly more efficient method for cleaning is not found.
Summary of the invention
For the cleaning of Macroscopic tissue heat acid attack corrosion product, there are the above problems, and the present invention is by hydrochloric acid, nitric acid to corrosion The solvability of product forms stronger cleaning gene with neopelex and combines, solves this technical problem.
To realize the above-mentioned technical purpose, used technical solution is: one kind is for clearing up the corrosion of steel macrostructure hot acid The cleaning agent of product, raw material are made of water, hydrochloric acid, nitric acid and neopelex, and the volume ratio of each raw material is water: salt Acid: nitric acid: neopelex=10:(0.1 ~ 5): (0.1 ~ 5): (0.01 ~ 5).
Cleaning agent of the present invention is by being water by the volume ratio of percent by volume, each raw material: hydrochloric acid: nitric acid: dodecane Base benzene sulfonic acid sodium salt=10:(0.1 ~ 5): (0.1 ~ 5): (0.01 ~ 5) is made after mixing.
Hydrochloric acid, nitric acid and neopelex of the present invention sequentially add in water.
The medicine have the advantages that
Hydrochloric acid, nitric acid and neopelex are combined, hydrochloric acid, nitric acid and neopelex is clear Clean soluble and undissolved dirt, the cleaning gene of the new Cheng Xin of triplicity, to achieve the purpose that effectively to clear up;Again because of salt Acid, nitric acid are carried out certain dilution by water, and are the tests carried out at normal temperature, while the time is not also grown, therefore will not be right Macrostructure result impacts.
Detailed description of the invention
Fig. 1 is GS-80 steel macrostructure figure;
Fig. 2 is preparation process figure of the invention;
Fig. 3 is 3% ~ 5% aqueous sodium carbonate to 35CrMoA macrostructure cleaning effect figure;
Fig. 4 is 10% ~ 15% aqueous solution of nitric acid to 35CrMoA macrostructure cleaning effect figure;
Fig. 5 is cleaning agent of the present invention to 35CrMoA macrostructure cleaning effect figure;
Fig. 6 is 2.5% nitric acid and 7.5% mixed in hydrochloric acid aqueous solution to 35CrMoA cleaning effect figure;
Fig. 7 is cleaning agent raw material of the present invention by volume successively to the effect picture after 35CrMoA cleaning;
Fig. 8 is 3% ~ 5% aqueous sodium carbonate to 45 steel macrostructure cleaning effect figures;
Fig. 9 is 10% ~ 15% aqueous solution of nitric acid to 45 macrostructure cleaning effect figures;
Figure 10 is cleaning agent of the present invention to 45 macrostructure cleaning effect figures;
Figure 11 is 2.5% nitric acid and 7.5% mixed in hydrochloric acid aqueous solution to 45 cleaning effect figures;
Figure 12 is cleaning agent raw material of the present invention by volume successively to the effect picture after 45 cleanings;
Figure 13 is 3% ~ 5% aqueous sodium carbonate to 05Cr17Ni4Cu4Nb steel macrostructure cleaning effect figure;
Figure 14 is 10% ~ 15% aqueous solution of nitric acid to 05Cr17Ni4Cu4Nb macrostructure cleaning effect figure;
Figure 15 is cleaning agent of the present invention to 05Cr17Ni4Cu4Nb macrostructure cleaning effect figure;
Figure 16 is 2.5% nitric acid and 7.5% mixed in hydrochloric acid aqueous solution to 05Cr17Ni4Cu4Nb cleaning effect figure;
Figure 17 is cleaning agent raw material of the present invention by volume successively to the effect picture after 05Cr17Ni4Cu4Nb cleaning;
Figure 18 is 3% ~ 5% aqueous sodium carbonate to GS-80 steel macrostructure cleaning effect figure;
Figure 19 is 10% ~ 15% aqueous solution of nitric acid to GS-80 macrostructure cleaning effect figure;
Figure 20 is cleaning agent of the present invention to GS-80 macrostructure cleaning effect figure;
Figure 21 is 2.5% nitric acid and 7.5% mixed in hydrochloric acid aqueous solution to GS-80 cleaning effect figure;
Figure 22 is cleaning agent raw material of the present invention by volume successively to the effect picture after GS-80 cleaning.
Specific embodiment
In technical solution, it is to solve the problems of dissolution of corrosion product first, is held under normal conditions using 3% ~ 5%( Product ratio) aqueous sodium carbonate or 10% ~ 15%(volumetric ratio) aqueous solution of nitric acid can dissolve corrosion product, but it is certain The corrosion product of Steel material is but difficult to thoroughly dissolve, so that influencing to grade to macrostructure accurate detection, sees Fig. 1, figure pilot scale The attachment of sample surface black is corrosion product.Grope and test by multiple, selection is by hydrochloric acid, nitric acid and ten in scheme Dialkyl benzene sulfonic acids sodium combines, and is cleaned.
Specific operating procedure is as follows:
A) cleaning agent, the formula of cleaning agent of the present invention are prepared according to new macrostructure cleaning agent formula are as follows:
Water (volume): hydrochloric acid (volume): nitric acid (volume): neopelex (volume)
=10:(0.1 ~ 5): (0.1 ~ 5): (0.01 ~ 5)
Above several liquid can be used after mixing.
B) the macrostructure sample after corroding to hot acid is brushed with a) prepared cleaning agent, and it is general to brush the time It is two minutes, is then rinsed with clear water, drying.
Experimental material is the Steel materials such as 35CrMoA, 45 steel, 05Cr17Ni4Cu4Nb, GS-80.
Experiment one will be pulled out with the good coarse micro-grain sample of hot acid (50% aqueous hydrochloric acid solution) etch, then with 3% ~ 5%(volume Than) aqueous sodium carbonate scrubbed, brushing time is 2 minutes, is then rinsed well and is dried up with clear water.
Experiment two re-works coarse micro-grain sample according to the requirement of GB/T 226-2015 to sample, then by sample Re-start hot acid erosion, hot acid lose it is good after sample is pulled out, with 10% ~ 15%(volumetric ratio) aqueous solution of nitric acid scrubbed, scrubbed Time is 2 minutes, is then rinsed well and is dried up with clear water.
Implement three, re-work coarse micro-grain sample to sample according to the requirement of GB/T 226-2015, then by sample Hot acid erosion is re-started, sample is pulled out after losing well, scrubbed with cleaning agent of the present invention by hot acid, and brushing time is 2 minutes, so It is rinsed well and is dried up with clear water afterwards.
Experiment four re-works coarse micro-grain sample according to the requirement of GB/T 226-2015 to sample, then by sample Hot acid erosion is re-started, sample is pulled out after losing well, scrubbed with 2.5% nitric acid and 7.5% mixed in hydrochloric acid aqueous solution by hot acid, is brushed Washing the time is 2 minutes, is then rinsed well and is dried up with clear water.
Experiment five re-works coarse micro-grain sample according to the requirement of GB/T 226-2015 to sample, then by sample Re-start hot acid erosion, hot acid lose it is good after sample is pulled out, by volume with cleaning agent raw material of the present invention, i.e. water (volume): salt Sour (volume)=10:(0.1 ~ 5), water (volume): nitric acid (volume)=10:(0.1 ~ 5), water (volume): neopelex (volume)=10:(0.01 ~ 5), it is successively scrubbed, brushing time is 2 minutes, is then rinsed well and is dried up with clear water.
Each experimental material is tested by above-mentioned steps, cleaning effect figure of five kinds of cleaning agents to experimental material Fig. 3-22 is seen respectively.
From being can be seen that in Fig. 3-12 for materials such as general steel alloy, carbon steels, the present invention clears up surface black corrosion The effect of product and conventional clean agent and 2.5%(volumetric ratio) cleaning of nitric acid and 7.5% (volumetric ratio) mixed in hydrochloric acid aqueous solution imitates Fruit is substantially suitable, more satisfactory, the mode that cleaning agent raw material of the present invention successively cleans by volume, and cleaning effect is clear not as good as this Lotion.
It can be seen that for Liang Zhongmashi figure stainless steel material from Figure 13-22, cleaning effect of the invention is bright It is aobvious better than traditional cleaning agent and 2.5%(volumetric ratio) nitric acid and 7.5% (volumetric ratio) mixed in hydrochloric acid aqueous solution and the present invention it is clear The mode that lotion raw material successively cleans by volume, so that macrostructure specimen surface more neat and tidy, ensure that low power The accuracy of tissue detection rating result.
Because cleaning agent of the present invention is after configuration is complete, solution becomes somewhat muddy by pellucidity, meanwhile, to list One cleaning and successively raw material cleaning comparison may determine that three kinds of main components in the present invention occur after mixing Certain reaction produces the efficient cleaning factor, and the ability of the cleaning factor dissolved corrosion product is relatively strong, can be more thorough Corrosion product is cleared up at bottom, reaches expected results of the invention, is not simply to combine the effect being anticipated that.

Claims (3)

1. a kind of for clearing up the cleaning agent of steel macrostructure hot acid corrosion product, it is characterised in that: to martensitic stain less steel The cleaning agent raw material that material is cleaned is made of water, concentrated hydrochloric acid, concentrated nitric acid and neopelex, the volume of each raw material Than for water: concentrated hydrochloric acid: concentrated nitric acid: neopelex=10:(0.1 ~ 5): (0.1 ~ 5): (0.01 ~ 5).
2. as described in claim 1 a kind of for clearing up the cleaning agent of steel macrostructure hot acid corrosion product, it is characterised in that: The cleaning agent is by being water by the volume ratio of percent by volume, each raw material: concentrated hydrochloric acid: concentrated nitric acid: neopelex =10:(0.1 ~ 5): (0.1 ~ 5): (0.01 ~ 5) is made after mixing.
3. as described in claim 1 a kind of for clearing up the cleaning agent of steel macrostructure hot acid corrosion product, it is characterised in that: Concentrated hydrochloric acid, concentrated nitric acid and the neopelex sequentially adds in water.
CN201610400889.1A 2016-06-08 2016-06-08 It is a kind of for clearing up the cleaning agent of steel macrostructure hot acid corrosion product Expired - Fee Related CN106086906B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102747368A (en) * 2012-06-27 2012-10-24 攀钢集团江油长城特殊钢有限公司 Etchant for maraging steel and examination method of maraging steel macrostructure
CN102914465A (en) * 2012-10-23 2013-02-06 鞍钢股份有限公司 TWIP (twinning induced plasticity) steel metallographic phase specimen preparation agent and use method thereof
CN103018141A (en) * 2012-11-29 2013-04-03 燕山大学 Original crystalline grain displaying agent of high-alloy and low-carbon martensite steel and displaying method
CN103510092A (en) * 2012-06-20 2014-01-15 鞍钢股份有限公司 Corrosion agent for displaying intercrystalline cracks of continuous casting steel billet and its preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103510092A (en) * 2012-06-20 2014-01-15 鞍钢股份有限公司 Corrosion agent for displaying intercrystalline cracks of continuous casting steel billet and its preparation method
CN102747368A (en) * 2012-06-27 2012-10-24 攀钢集团江油长城特殊钢有限公司 Etchant for maraging steel and examination method of maraging steel macrostructure
CN102914465A (en) * 2012-10-23 2013-02-06 鞍钢股份有限公司 TWIP (twinning induced plasticity) steel metallographic phase specimen preparation agent and use method thereof
CN103018141A (en) * 2012-11-29 2013-04-03 燕山大学 Original crystalline grain displaying agent of high-alloy and low-carbon martensite steel and displaying method

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