CN104749125A - Detection method of residual carbon content on cold rolled steel sheet surface - Google Patents

Detection method of residual carbon content on cold rolled steel sheet surface Download PDF

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Publication number
CN104749125A
CN104749125A CN201310726534.8A CN201310726534A CN104749125A CN 104749125 A CN104749125 A CN 104749125A CN 201310726534 A CN201310726534 A CN 201310726534A CN 104749125 A CN104749125 A CN 104749125A
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China
Prior art keywords
sample
rolled steel
cold
carbon
steel sheet
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CN201310726534.8A
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Chinese (zh)
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宋旭飞
陆伟星
王鑫艳
王海军
周桂海
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Shanghai Meishan Iron and Steel Co Ltd
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Shanghai Meishan Iron and Steel Co Ltd
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Abstract

The invention relates to a detection method of the residual carbon content on a cold rolled steel sheet surface, and mainly solves the technical problem that the prior art can not detect residual carbon content on the cold rolled steel sheet surface. A technical proposal of the invention is as below: sampling by continuously intercepting three pieces of samples on a cold rolled steel sheet without pollution or corrosion; sample preparation by clipping an analysis sample in the size of 2.5 cm*10 cm or 2.0 cm * 12.5 cm from the selected sample; placing the sample in a caranalyzer, controlling the temperature in the caranalyzer at 600 DEG C-670 DEG and introducing oxygen for 200-480 s with oxygen flow at 2-3 L / min, and determining carbon content in carbon dioxide gas by the caranalyzer; and calculating the residual carbon content on the sample surface. The determination method of the invention can accurately determine the residual carbon content on the cold-rolled steel sheet in only 30 minutes, and the accuracy can reach 1.0 mg / m<2>, so as to provide the basis for the judgment of the cleanliness of the cold rolled steel sheet surface.

Description

A kind of detection method of surface of cold-rolled steel plate remaining carbon
 
Technical field
The invention belongs to field of metal material detection, relate to the detection method of surface of cold-rolled steel plate composition, particularly a kind of detection method of surface of cold-rolled steel plate remaining carbon, the judgement being mainly surface of cold-rolled steel plate cleanliness provides foundation.
Background technology
In recent years, China Automobile Industry, household electric appliances, the demand of wrapping enterprise to cold-rolled steel sheet continue to increase, and the surface quality requirements of user to cold-rolled steel sheet also improves constantly.The index of surface of cold-rolled steel plate cleanliness becomes a decisive indicator of market competition gradually.The residue of surface of steel plate can make surface passivation process bring difficulty, uneven coating can occur, affect the adhesion of coating, and belt steel surface produces and burns point, some rust, grey black etc., reduces the surface quality of steel plate.
After cold-rolled steel sheet rolling, coating front surface with the material such as ROLLING OIL, railway grease, emulsifying agent, leveling precision, these materials are commonly referred to as Residual oil.Long chain hydrocarbon in Residual oil starts cracking through high temperature, separates out active atoms of carbon and is adsorbed onto surface of steel plate and is combined into carbon molecule deposition and gets off, be called carbon residue.Surface of cold-rolled steel plate cleanliness are mainly weighed with surface residue content.Generally weigh with indexs such as Oil residue on surface, residual iron, remaining carbons.
The method correlation technique detecting surface of cold-rolled steel plate cleanliness is many, Chinese patent CN 101354329 B, name is called, a kind of total residual of belt steel surface and the measuring method of residual ferrous powder, disclose the measuring method of a kind of surface of steel plate total residual and residual iron, the method uses chemical solvents such as the virulent butanone of human body, there is the potential hazard to environment, and method of operating is unfavorable for standardization, the accuracy of detection few for surface of cold-rolled steel plate residue can not ensure, sample easily causes testing result distortion.
Chinese patent CN 102033002 A, name is called, a kind of detection method of surface residual oil quantity of rolled cold-rolling steel sheet, disclose, a detection method for cold-rolled steel sheet residua content after rolling, mainly there is following several respects problem in the method: (1) needs special extraction equipment, and relate to a large amount of poisonous and hazardous chemical reagent, be unfavorable for that operating personnel are healthy, be more unfavorable for environmental protection of enterprise production requirement.(2) process is loaded down with trivial details, complicated operation, and the detection generally completing one group of surface residual oil quantity of rolled cold-rolling steel sheet needs 8 hours, is difficult to meet the requirement of modern enterprise fast pace.(3) most of action need manual operations, is difficult to realize automation mechanized operation.(4) amount of samples is too large, and produce pressure to on-site sampling, product causes waste.(5) understanding detection method range of results from experimental data is 300-500mg/m2, and after being only applicable to rolling, the Residual oil on annealing front spring surface, to after annealing, oleaginousness is lower than the steel plate of 20mg/m2, and the weighing error of the method can cause result inaccurate.
Ultimate principle disclosed in prior art or organic solvent soaking extraction-gravimetric method.The major defect of gravimetric determination Residual oil has two, one is the restriction by weighing error, generally be only applicable to the detection of high level (generally at more than 100mg/m2) Residual oil, otherwise random error is larger, two is the restrictions by cleaning method, effects on surface hydrocarbon responds, and after annealing, uncombined carbon cannot clean, therefore can not reflect the state of surface residue comprehensively.
Surface of cold-rolled steel plate residual carbon content can reflect surface of steel plate cleanliness intuitively, and prior art does not also have the detection method of surface of cold-rolled steel plate residual carbon content at present.Cold rolling electroplating tinbase plate is the cold-rolled steel sheet that quality is higher, and its Oil residue on surface is at about 20mg/m2, and after cleaning, plate is lower, and known method is also inapplicable.Be badly in need of the fast and convenient measurement means setting up a kind of Accurate Determining surface of cold-rolled steel plate remaining carbon, improving for carrying out surface of cold-rolled steel plate cleanliness, providing the plate surface quality index of quantification, Improving The Quality of Products, reducing user quality objection provides detection means.
Summary of the invention
The object of this invention is to provide a kind of detection method of surface of cold-rolled steel plate remaining carbon, solve the technical matters that in prior art, surface of cold-rolled steel plate carbon residue cannot detect, for the judgement of surface of cold-rolled steel plate cleanliness provides foundation.
The technical solution used in the present invention is:
A detection method for surface of cold-rolled steel plate remaining carbon, comprises the following steps:
A, sampling, the cold-rolled steel sheet of pollution-free, non-corroding intercepts three pieces of samples continuously, every block specifications: long × wide be 15cm × 10cm, and after intercepting, overlap lies in together successively, chooses the sample overlaying centre during detection;
B, sample preparation, the analysis sample of clip 2.5cm × 10cm or 2.0cm × 12.5cm from the sample chosen, each sample produces more than three; The rectangle sample made is processed into [shape, two ends vertical plane is bending 0.5cm or 1.0cm upwards;
C, sample is positioned in carbometer, control temperature in carbometer be 600 DEG C ~ 670 DEG C and lead to oxygen 200 seconds ~ 480 seconds, oxygen flow is 2 ~ 3L/min, makes the carbon residue of sample surfaces change carbon dioxide into, measures carbon content in carbon dioxide with carbometer;
D, calculate specimen surface remaining carbon.
 
In step a of the present invention, the sample after intercepting successively overlap keeps flat, and chooses and overlay middle sample during measurement, being the pollution for reducing to greatest extent to sample in sampling and handling process, increasing the accuracy of data.
In step c of the present invention, in carbometer, logical oxygen, under cold-rolled steel sheet sample for guaranteeing to be placed in carbometer is in oxygen-enriched atmosphere, because under oxygen-enriched atmosphere, cold-rolled steel sheet is heated to certain degree Celsius, surface of steel plate carbon residue all will change into carbon dioxide, then measures its carbon amounts with carbometer.
Again, in step c, before to sample analysis, first standard correction is carried out to carbometer, after carry out sample analysis, often organize sample analysis more than three, analysis result is averaged;
Further, steps d, calculates specimen surface remaining carbon by formula one:
(formula one)
In formula one, C (surface)for carbon contents in sample, mg/m 2; M is carbon content in carbometer working sample, and unit is mg; S is determined region area, and unit is m 2.
The present invention is by adopting sample preparation, testing conditions controls, eliminate the interference that the inner carbon of sampling error and steel plate measures for carbon residue, adopt infrared absorption determining surface of steel plate carbon (comprising hydrocarbon and agraphitic carbon) content, detect while realizing Residual oil and other uncombined carbons, solving surface of cold-rolled steel plate remaining carbon cannot a detection technique difficult problem, simultaneously for the surface of cold-rolled steel plate cleanliness indexs such as the electric tinbase plate of cold rolling plating judge to provide foundation.
According to the sign that the carbon residue content of the present invention's mensuration is steel plate cleanliness, measure the cleanliness of steel plate, steel substrate cleaning performance can be evaluated more clearly, contribute to improving coated plate surface quality.
The present invention has following good effect compared to existing technology:
1. present invention achieves surface of cold-rolled steel plate carbon residue rapid and accurate determination, easy and simple to handle, labour intensity is low, it is high to detect automaticity, testing same group of surface of steel plate residual carbon content time is about 30min.
2. the present invention characterizes the total amount of cold rolled surface residue by measuring surface of cold-rolled steel plate carbon amounts, and more accurately comprehensively, the cold-rolled steel sheet very low to annealing rear surface residue, detects precision high, can be accurate to 1.0mg/m testing result 2carbon content.
3. the present invention is without the need to using poisonous and harmful reagent, is conducive to the healthy of testing staff, reduces human body and environmental hazard, environmental protection of enterprise demand for development.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Accompanying drawing 1 intercepts the disposing way schematic diagram of sample for the present invention
The front view of the sample that accompanying drawing 2 prepares for the present invention
Description of symbols in figure:
1-cover plate; 2-steel plate to be measured; 3-base plate; The sample that 4-prepares;
Embodiment
A detection method for surface of cold-rolled steel plate remaining carbon, comprises the following steps:
A, sampling, the cold-rolled steel sheet of pollution-free, non-corroding intercepts three pieces of samples continuously, every block specifications: long × wide be 15cm × 10cm, and after intercepting, overlap lies in together successively, see Fig. 1, chooses the sample overlaying centre during detection;
B, sample preparation, the analysis sample of clip 2.5cm × 10cm from the sample chosen, each sample produces three; The rectangle sample plate shearing machine made is processed into [shape, see Fig. 2, two ends vertical plane is bending 0.5cm upwards;
C, sample is positioned over model is SC144, in the carbometer that Leco Corporation of the U.S. manufactures, controls temperature in carbometer and is 600 DEG C and logical oxygen 200 seconds, oxygen flow is 2 ~ 3L/min, measure carbon content in carbon dioxide with carbometer afterwards, often organize sample analysis three, analysis result is averaged;
D, calculate specimen surface remaining carbon by formula one:
(formula one)
In formula one, C (surface)for carbon contents in sample, mg/m 2; M is carbon content in carbometer working sample, and unit is mg; S is determined region area, and unit is m 2.
Again, in step c, also comprise before to sample analysis and standard correction is carried out to carbometer, take synthesis carbon standard substance (502-029), analyze carbon content by carbometer, repeat 3 times, standard correction carbometer.
The preci-sion and accuracy of the inventive method is confirmed by the recovery testu of sample and Precision Experiment.
Recovery experiment, after sample surface of cold-rolled steel plate drips certain gauging, by the inventive method, the recovery of standard addition of test samples, test findings sees the following form 1.
Table 1 sample recovery testu
Be added dropwise to oil mass (g) Yield (g) The recovery (%)
0.1001 0.0999 99.8
0.2025 0.2030 100.2
0.3005 0.2966 98.7
0.4003 0.3990 99.7
Precision Experiment, carry out 11 Precision Experiments to 2 groups of cold-rolled steel sheets, analysis result sees the following form 2.
Table 2 sample Precision Experiment
Above-mentioned experimental result shows, in the recovery testu of sample, the surface of cold-rolled steel plate residual carbon content recovery is between 99.7 ~ 100.2%, and the recovery is higher, RSD is less than 3%, detect data precision good, prove that the inventive method accurately and reliably, meet iron and steel enterprise's production requirement completely.

Claims (2)

1. a detection method for surface of cold-rolled steel plate remaining carbon, is characterized in that, said method comprising the steps of:
A, sampling, the cold-rolled steel sheet of pollution-free, non-corroding intercepts three pieces of samples continuously, every block specifications: long × wide be 15cm × 10cm, and after intercepting, overlap lies in together successively, chooses the sample overlaying centre during detection;
B, sample preparation, the analysis sample of clip 2.5cm × 10cm or 2.0cm × 12.5cm from the sample chosen, each sample produces more than three; The rectangle sample made is processed into [shape, two ends vertical plane is bending 0.5cm or 1.0cm upwards;
C, be positioned in carbometer by sample, control temperature in carbometer and be 600 DEG C ~ 670 DEG C and logical oxygen 200 seconds ~ 480 seconds, oxygen flow is 2 ~ 3L/min, and rear carbometer measures carbon content in carbon dioxide;
D, calculate specimen surface remaining carbon.
2. the detection method of a kind of surface of cold-rolled steel plate remaining carbon as claimed in claim 1, is characterized in that, calculate specimen surface remaining carbon in described steps d by formula one:
(formula one)
In formula one, C (surface)for carbon contents in sample, mg/m 2; M is carbon content in carbometer working sample, and unit is mg; S is determined region area, and unit is m 2.
CN201310726534.8A 2013-12-26 2013-12-26 Detection method of residual carbon content on cold rolled steel sheet surface Pending CN104749125A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108181158A (en) * 2017-12-28 2018-06-19 广州大学 A kind of detection method of cold rolling workpiece rolling rear surface resid amount
CN111678912A (en) * 2020-06-18 2020-09-18 武汉钢铁有限公司 Method for measuring residual carbon content on surface of cold-rolled sheet

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CN101329242A (en) * 2008-08-05 2008-12-24 株洲硬质合金集团有限公司 Method for analyzing and detecting free carbon in chromium carbide
CN101581650A (en) * 2009-06-01 2009-11-18 中国铝业股份有限公司 Method for measuring organic carbon content in sodium aluminate serosity
CN102313664A (en) * 2010-06-29 2012-01-11 鞍钢股份有限公司 Surface treatment method of ultra-low carbon content sheet sample
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108181158A (en) * 2017-12-28 2018-06-19 广州大学 A kind of detection method of cold rolling workpiece rolling rear surface resid amount
CN111678912A (en) * 2020-06-18 2020-09-18 武汉钢铁有限公司 Method for measuring residual carbon content on surface of cold-rolled sheet
CN111678912B (en) * 2020-06-18 2023-12-12 武汉钢铁有限公司 Method for measuring residual carbon content on surface of cold-rolled sheet

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Application publication date: 20150701