CN106840822B - A kind of surface treatment method measuring stainless oxygen content in steel sample - Google Patents
A kind of surface treatment method measuring stainless oxygen content in steel sample Download PDFInfo
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- CN106840822B CN106840822B CN201710221381.XA CN201710221381A CN106840822B CN 106840822 B CN106840822 B CN 106840822B CN 201710221381 A CN201710221381 A CN 201710221381A CN 106840822 B CN106840822 B CN 106840822B
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- pickling solution
- stainless steel
- oxygen content
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
Abstract
The present invention relates to determination of oxygen content technical field in stainless steel, the surface treatment method of specifically a kind of stainless oxygen content in steel sample of measurement.Stainless steel granular is through first step pickling, and oxidation-reduction is in the second step pickling solution processing of equilibrium state (activate and partial deactivation process is in periodically to act on sample surfaces), the compact oxidation layer that can quickly form each kind stainless steel due to high-temperature oxydation in mechanical processing process is completely, thoroughly clean up, and sample surfaces anacidity washing lotion and other impurity remain, and can timely and accurately provide the percentage composition of trace oxygen in melting finished product sample by PULSE HEATING inert gas fusion-infrared absorption.
Description
Technical field
The present invention relates to determination of oxygen content technical field in stainless steel, specifically a kind of stainless oxygen content in steel sample of measurement
Surface treatment method.
Background technique
Oxygen is a kind of harmful element in steel, and oxygen content in steel is the important indicator of steel product quality quality.Oxygen master in steel
To exist in the form that oxide is mingled with, such as: Al2O3, SiO2, MnO, FeO.Since non-metallic inclusion (oxide) destroys
The continuity of metal structure even if content is very low can also make the degradation of steel, such as shock resistance, fatigue resistance
The deterioration of energy.In order to reduce oxygen content in steel, steel cleanliness is improved, promotes steel physical property, it is accurate, fast in smelting process
Speed measurement trace oxygen content is just particularly important.
The common and reliable method of determination of oxygen content is exactly PULSE HEATING inert gas fusion --- infrared absorption,
This method requires sample to be tested specific surface area to want small, general to require to be that surface no-pollution, metallic matrix are exposed, clean granular
Sample.The oxide layer and the depth that the preparation process of sample will make sample surfaces form uneven thickness when both analysis oxygen content
Different mechanical scratch is unable to satisfy analysis method to sample surfaces light, cleanliness requirement, therefore, can only become a useful person before this in steel
Taken afterwards by special sample processing procedure, sample preparation, oxygen content could be measured, take, sample preparation and analytical cycle it is longer, can not be timely
Instructing manufacture, and directly affect steel product quality and determine the period.
Chemical method cleaning is the removal effective method of oxidation on metal surface layer, is existed in oxide layer on stainless steel surface
The sharp crystalline structure compound of FeO, Cr2O3, are difficult to dissolve, and very fine and close, pickling solution is not easy to permeate.
Summary of the invention
The technical problems to be solved by the present invention are: how quickly to remove the surface of surely stainless oxygen content in steel sample.
The technical scheme adopted by the invention is that: a kind of surface treatment method measuring stainless oxygen content in steel sample is pressed
It is carried out according to following steps
Step 1: the first pickling solution of configuration and the second pickling solution, the first pickling solution is by ferric trichloride FeCl3, hydrochloric acid HCl,
Triethanolamine TEOA, polyethylene glycol PEG-600, water composition, wherein ferric trichloride mass percentage content is 10-15%, HCl's
Molecular number is FeCl36-7 times of molecular number, triethanolamine TEOA and polyethylene glycol PEG-600 are shared in the first pickling solution
Volume fraction is between 1%-3%, and the second pickling solution is by oxalic acid H2C2O4, hydrogen peroxide H2O2, water composition, wherein oxalic acid H2C2O4
Mass percentage content be 30%, H2O2Molecular number be H2C2O43 times of molecular number；
Step 2: the stainless steel particulate samples that surface has been oxidized to be put into 90-100 DEG C of the first pickling solution, constant temperature
It impregnates 5 minutes, takes out stainless steel particulate samples, after distilled water cleans 2 times, then put into 50-60 DEG C of the second pickling solution, then set
It is cleaned 1.5 minutes in supersonic wave cleaning machine, takes out stainless steel particulate samples, distilled water cleans 4-5 times, after hair dryer drying, even
It is continuous to pass through washes of absolute alcohol twice, finally reuse hair dryer drying.
The beneficial effects of the present invention are: oxidisability of the invention patent by ferric ion, nonionic surfactant
Infiltration permeability, while using triethanolamine corrosion inhibition, particulate samples surface oxide layer is quickly removed, is dissolved, is made
Metallic matrix is exposed, and the sample surfaces clean situation for preparing stokehold meets oxygen analysis method (GB/T11261-2006 steel
Measurement PULSE HEATING inert gas fusion --- the infrared absorption of iron oxygen content) it requires, realizing can be accurate, fast in stokehold
Speed measurement oxygen content, instructs smelting process for production, shortens steel product quality and determines the period, increases economic efficiency.Specially using non-
The wellability and Penetration Signature that ionic surface active agent --- polyethylene glycol (PEG) -600 provides, enhance the penetration of pickling solution.
Under the premise of Action of Surfactant, using the oxidisability of iron chloride, oxidation-reduction reaction occurs with iron in sample matrices:
2FeCl3+Fe=3FeCl2 is conducive to the removing of oxide layer so that generating gap between oxide layer and matrix.Using reproducibility without
Machine acid --- hydrochloric acid, on the one hand for being partly dissolved epidermis oxide, on the other hand can be prevented as main pickling liquid medium
The hydrolysis for the ferrous ion that ferric ion and reaction generate.A certain amount of triethanolamine (TEOA) corrosion inhibiter, control acid is added
Reaction process is washed, spot corrosion and excessive erosion of the pickling solution to sample surfaces are avoided.It is (living in equilibrium state using oxidation-reduction
Change and partial deactivation process be in periodically act on sample surfaces) second step pickling solution --- oxalic acid+mistake of suitable proportion
Hydrogen peroxide solution ultrasonication sample, by attachment that first step pickling is formed quickly, thoroughly remove.
Specific embodiment
A kind of surface treatment method measuring stainless oxygen content in steel sample,
Configure the first pickling solution: by 10~15g ferric trichloride be dissolved in 100mL concentration be 6~9mol/L hydrochloric acid solution in,
Make the molecular number FeCl of HCl36 times of molecular number add triethanolamine (TEOA) and polyethylene glycol (PEG-600), three second
Volume fraction hydramine TEOA and polyethylene glycol PEG-600 shared in the first pickling solution is between 1%-3%, after solution mixes
For use.
Configure the second pickling solution: by dissolving oxalic acid in the hydrogenperoxide steam generator prepared by commercially available hydrogen peroxide, oxalic acid is dense
Degree should be lower than its solubility at normal temperature, oxalic acid H2C2O4Mass percentage content be 30%, H2O2Molecular number be H2C2O4
3 times of molecular number.
By after machining, stainless steel granular that the quality that surface has been oxidized is about 1g or so (column, spherical or circle
Pie etc.) investment is heated to 90-100 DEG C of the first pickling solution, and constant temperature impregnates 5 minutes, takes out sample particle, distilled water cleaning 2
After secondary, then the second pickling solution (50-60 DEG C) is put into, is placed in supersonic wave cleaning machine together with beaker and cleans 1.5 minutes, take out sample
Grain, distilled water clean 4-5 times, after hair dryer is dry, continuously across washes of absolute alcohol twice, use arteries and veins in time after hair dryer is dry
Oxygen content in punching heating one infrared absorption of inert gas fusion measurement sample.
Pickling of the present invention is high-efficient, in a short period of time can clean up the oxide layer that machining generates, acid
Rear sample surfaces are washed without any residual.The requirement that can satisfy steel-making both analysis trace oxygen content, reaches timely guidance
The purpose of production.Can pickling stainless steel kind it is extensive, including chromium-stainless steel, chromium-nickel and stainless steel, such as: 400 be stainless steel,
300 be stainless steel, heat-resistance stainless steel and two phase stainless steel etc..Input cost is low, pollutes small, the sustainable use of pickling solution.Acid
The equipment that washed journey uses is simple, and operating process is easy.
Claims (1)
1. a kind of surface treatment method for measuring stainless oxygen content in steel sample, it is characterised in that: carry out in accordance with the following steps
Step 1: the first pickling solution of configuration and the second pickling solution, the first pickling solution is by ferric trichloride FeCl3, hydrochloric acid HCl, three ethyl alcohol
Amine TEOA, polyethylene glycol PEG-600, water composition, wherein ferric trichloride mass percentage content is 10-15%, the molecular number of HCl
For FeCl3Volume point 6-7 times of molecular number, triethanolamine TEOA and polyethylene glycol PEG-600 shared in the first pickling solution
Number is between 1%-3%, and the second pickling solution is by oxalic acid H2C2O4, hydrogen peroxide H2O2, water composition, wherein oxalic acid H2C2O4Quality
Degree is 30%, H2O2Molecular number be H2C2O43 times of molecular number；
Step 2: the stainless steel particulate samples that surface has been oxidized to be put into 90-100 DEG C of the first pickling solution, constant temperature impregnates 5
Minute, stainless steel particulate samples are taken out, after distilled water cleans 2 times, then 50-60 DEG C of the second pickling solution is put into, is subsequently placed in super
Sound wave cleaning machine cleans 1.5 minutes, takes out stainless steel particulate samples, and distilled water cleans 4-5 times, continuous to pass through after hair dryer drying
After washes of absolute alcohol twice, hair dryer drying is finally reused.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710221381.XA CN106840822B (en) | 2017-04-06 | 2017-04-06 | A kind of surface treatment method measuring stainless oxygen content in steel sample |
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| CN201710221381.XA CN106840822B (en) | 2017-04-06 | 2017-04-06 | A kind of surface treatment method measuring stainless oxygen content in steel sample |
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| CN106840822A CN106840822A (en) | 2017-06-13 |
| CN106840822B true CN106840822B (en) | 2019-11-01 |
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| CN110530704A (en) * | 2019-08-13 | 2019-12-03 | 中航金属材料理化检测科技有限公司 | The chemical pre-processing method of oxygen and nitrogen content in a kind of measurement steel |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203320132U (en) * | 2013-05-30 | 2013-12-04 | 天津市顺通带钢有限公司 | Pickler |
| CN105908197A (en) * | 2016-06-22 | 2016-08-31 | 山西艾尔德添加剂新技术有限公司 | Pickling additive for surface oxide scale of stainless steel material and preparation method therefor and pickling method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203320132U (en) * | 2013-05-30 | 2013-12-04 | 天津市顺通带钢有限公司 | Pickler |
| CN105908197A (en) * | 2016-06-22 | 2016-08-31 | 山西艾尔德添加剂新技术有限公司 | Pickling additive for surface oxide scale of stainless steel material and preparation method therefor and pickling method thereof |
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