CN106840822A - A kind of surface treatment method for determining stainless oxygen content in steel sample - Google Patents
A kind of surface treatment method for determining stainless oxygen content in steel sample Download PDFInfo
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- CN106840822A CN106840822A CN201710221381.XA CN201710221381A CN106840822A CN 106840822 A CN106840822 A CN 106840822A CN 201710221381 A CN201710221381 A CN 201710221381A CN 106840822 A CN106840822 A CN 106840822A
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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
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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
- G01N1/34—Purifying; Cleaning
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Abstract
The present invention relates to determination of oxygen content technical field in stainless steel, specifically a kind of surface treatment method for determining stainless oxygen content in steel sample.Stainless steel granular is through first step pickling, and redox is in poised state（Activation and partial deactivation process are in periodically to act on sample surfaces）Second step pickle treatment, can quickly by each kind stainless steel in mechanical processing process due to high-temperature oxydation formed compact oxidation layer is complete, thoroughly cleaning is clean, and sample surfaces anacidity washing lotion and other impurities lefts, the percentage composition of trace oxygen in melting finished product sample can be timely and accurately provided by PULSE HEATING inert gas fusion infrared absorption.
Description
Technical field
It is specifically a kind of to determine stainless oxygen content in steel sample the present invention relates to determination of oxygen content technical field in stainless steel
Surface treatment method.
Background technology
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 of oxide is mingled with, such as：Al2O3, SiO2, MnO, FeO etc..Due to non-metallic inclusion（Oxide）Destruction
The continuity of metal structure, even if content is very low, can also cause the degradation of steel, such as shock resistance, fatigue resistance
The deterioration of energy.In order to reduce oxygen content in steel, steel cleanliness factor is improved, lift steel physical property, it is accurate in smelting process, fast
Speed determines trace oxygen content and is just particularly important.
The conventional and reliable method of determination of oxygen content is exactly PULSE HEATING inert gas fusion --- infrared absorption,
The method requirement testing sample specific surface area is small, general to require as surface no-pollution, metallic matrix are exposed, cleaning granular
Sample.The preparation process of sample will make sample surfaces form the oxide layer and the depth of uneven thickness during both analysis oxygen content
The mechanical mark for differing, it is impossible to meet analysis method to sample surfaces light, cleanliness requirement, therefore, can only be become a useful person in steel before this
Taken by special sample processing procedure afterwards, sample preparation, oxygen content could be determined, take, sample preparation and analytical cycle it is more long, it is impossible in time
Instructing manufacture, and directly affect the steel product quality judgement cycle.
Chemical method cleaning is the removal oxidation on metal surface effective method of layer, is existed in oxide layer on stainless steel surface
The sharp crystalline structure compound of FeO, Cr2O3, it is difficult to dissolve, and it is very fine and close, pickle is difficult infiltration.
The content of the invention
The technical problems to be solved by the invention are：How the surface of surely stainless oxygen content in steel sample is quickly removed.
The technical solution adopted in the present invention is：A kind of surface treatment method for determining stainless oxygen content in steel sample, presses
Carried out according to following steps
Step one, configuration the first pickle and the second pickle, the first pickle is by ferric trichloride FeCl3, hydrochloric acid HCl, three second
Hydramine TEOA, polyethylene glycol PEG-600, water composition, wherein, ferric trichloride mass percentage content is 10-15%, the molecule of HCl
Number is FeCl36-7 times of molecular number, triethanolamine TEOA and the shared volumes in the first pickle of polyethylene glycol PEG-600
Between 1%-3%, the second pickle is by oxalic acid H for fraction2O2, hydrogen peroxide H2C2O4, water composition, wherein, oxalic acid H2O2Matter
Amount degree is 30%, H2O2Molecular number be H2C2O43 times of molecular number；
Step 2, the stainless steel particulate samples for being oxidized surface put into 90-100 DEG C of the first pickle, constant temperature immersion 5
Minute, stainless steel particulate samples are taken out, after distilled water cleans 2 times, then 50-60 DEG C of the second pickle is put into, it is subsequently placed in super
Sound wave cleaning machine is cleaned 1.5 minutes, takes out stainless steel particulate samples, and distilled water is cleaned 4-5 times, after hair-dryer drying, continuous warp
After washes of absolute alcohol twice, hair-dryer drying is finally reused.
The beneficial effects of the invention are as follows：Oxidisability, nonionic surfactant of the patent of the present invention by ferric ion
Infiltration permeability, while using the corrosion inhibition of triethanolamine, particulate samples surface oxide layer quickly being peeled off, being dissolved, make
Metallic matrix is exposed, and the sample surfaces clean situation for preparing stokehold meets oxygen analysis method（GB/T11261-2006 steel
Measure PULSE HEATING inert gas fusion --- the infrared absorption of iron oxygen content）It is required that, realizing just can be accurate, fast in stokehold
Speed determines oxygen content, instructs smelting process for production, shortens steel product quality and judges the cycle, increases economic efficiency.Specially using non-
Ionic surface active agent --- polyethylene glycol（PEG）- 600 wellabilities and Penetration Signature for providing, strengthen the penetration of pickle.
On the premise of Action of Surfactant, using the oxidisability of iron chloride, there is oxidation-reduction reaction with iron in sample matrices：
2FeCl3+Fe=3FeCl2 so that gap is produced between oxide layer and matrix, is conducive to the stripping of oxide layer.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 of ferric ion and the ferrous ion of reaction generation.Add a certain amount of triethanolamine（TEOA）Corrosion inhibiter, control acid
Wash reaction process, it is to avoid spot corrosion and excessive erosion of the pickle to sample surfaces.It is in poised state using oxidation-reduction（It is living
Change and partial deactivation process is in periodically to act on sample surfaces）Second step pickle --- the oxalic acid+mistake of suitable proportion
Hydrogen peroxide solution ultrasonication sample, the attachment that first step pickling is formed is quick, thoroughly removing.
Specific embodiment
A kind of surface treatment method for determining stainless oxygen content in steel sample,
Configure the first pickle：10~15g ferric trichlorides are dissolved in 100mL concentration in 6~9mol/L hydrochloric acid solutions, to make
The molecular number of HCl is FeCl36 times of molecular number, add triethanolamine（TEOA）And polyethylene glycol（PEG-600）, three ethanol
Between 1%-3%, solution is treated after mixing for amine TEOA and the shared volume fractions in the first pickle of polyethylene glycol PEG-600
With.
Configure the second pickle：By dissolving oxalic acid in the hydrogenperoxide steam generator prepared by commercially available hydrogen peroxide, oxalic acid is dense
Degree should be less than its solubility at normal temperatures, oxalic acid H2O2Mass percentage content be 30%, H2O2Molecular number be H2C2O4Point
3 times of subnumber.
By after machining, the stainless steel granular of quality about 1g or so that has been oxidized of surface（Column, spherical or circle
Pie etc.）Input is heated to 90-100 DEG C of the first pickle, and constant temperature soaks 5 minutes, takes out sample particle, distilled water cleaning 2
After secondary, then put into the second pickle（50-60℃）, it is placed in supersonic wave cleaning machine together with beaker and cleans 1.5 minutes, take out sample
Grain, distilled water is cleaned 4-5 times, and after hair-dryer is dried, continuously across washes of absolute alcohol twice, hair-dryer uses arteries and veins in time after drying
Oxygen content in the punching heating infrared absorption determination sample of inert gas fusion one.
Pickling efficiency high of the present invention, can will just be machined the oxide layer for producing and clean up in a short period of time, acid
Rear sample surfaces are washed without any residual.The requirement of steel-making both analysis trace oxygen content is disclosure satisfy that, guidance in time is reached
The purpose of production.Can pickling stainless steel kind extensively, including chromium-stainless steel, chromium-nickel and stainless steel, such as：400 be stainless steel,
300 is stainless steel, heat-resistance stainless steel and two phase stainless steel etc..Input cost is low, pollutes small, and pickle is sustainable to be used.Acid
The equipment that washed journey is used is simple, and operating process is easy.
Claims (1)
1. a kind of surface treatment method for determining stainless oxygen content in steel sample, it is characterised in that：Carry out in accordance with the following steps
Step one, configuration the first pickle and the second pickle, the first pickle is by ferric trichloride FeCl3, hydrochloric acid HCl, three ethanol
Amine TEOA, polyethylene glycol PEG-600, water composition, wherein, ferric trichloride mass percentage content is 10-15%, the molecular number of HCl
It is FeCl36-7 times of molecular number, triethanolamine TEOA and the shared volume integrals in the first pickle of polyethylene glycol PEG-600
Between 1%-3%, the second pickle is by oxalic acid H for number2O2, hydrogen peroxide H2C2O4, water composition, wherein, oxalic acid H2O2Quality
Degree is 30%, H2O2Molecular number be H2C2O43 times of molecular number；
Step 2, the stainless steel particulate samples for being oxidized surface put into 90-100 DEG C of the first pickle, constant temperature immersion 5
Minute, stainless steel particulate samples are taken out, after distilled water cleans 2 times, then 50-60 DEG C of the second pickle is put into, it is subsequently placed in super
Sound wave cleaning machine is cleaned 1.5 minutes, takes out stainless steel particulate samples, and distilled water is cleaned 4-5 times, after hair-dryer drying, continuous warp
After washes of absolute alcohol twice, hair-dryer drying is finally reused.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| 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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| CN106840822A true CN106840822A (en) | 2017-06-13 |
| CN106840822B CN106840822B (en) | 2019-11-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115656146A (en) * | 2022-10-17 | 2023-01-31 | 山西太钢不锈钢股份有限公司 | Method for measuring silver content in antibacterial stainless 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 |
-
2017
- 2017-04-06 CN CN201710221381.XA patent/CN106840822B/en active Active
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 |
Non-Patent Citations (1)
| Title |
|---|
| 黄玉媛 等: "《精细化学品实用配方手册》", 31 January 2009, 中国纺织出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115656146A (en) * | 2022-10-17 | 2023-01-31 | 山西太钢不锈钢股份有限公司 | Method for measuring silver content in antibacterial stainless steel |
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| Publication number | Publication date |
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| CN106840822B (en) | 2019-11-01 |
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