CN100451602C - Preparation method of steel sample for determining component content in steel - Google Patents
Preparation method of steel sample for determining component content in steel Download PDFInfo
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- CN100451602C CN100451602C CNB2006100129268A CN200610012926A CN100451602C CN 100451602 C CN100451602 C CN 100451602C CN B2006100129268 A CNB2006100129268 A CN B2006100129268A CN 200610012926 A CN200610012926 A CN 200610012926A CN 100451602 C CN100451602 C CN 100451602C
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Abstract
The present invention relates to preparation method of an element test sample in steel, which comprises the following procedures that I, a test sample is taken from a ladle, the obtained test sample forms a rod shape, the taper of the rod-shaped test sample is from 0 to 0.4 and is used for guaranteeing that when the test sample is cut, the thicknesses of both a head and a tail are respectively larger than 10mm, and the thickness in the middle position of the test sample is more than 6mm; II, the test sample is cut, and the rod-shaped test sample is clamped by a clamp so as to cut out sheet test samples, of which the thickness is not less than 6mm; III, two surfaces of each sheet test sample is processed, a plane processing device is used for processing the positive and the negative planes of the sheet test sample, and the value of the surface roughness of the surface of the processed sheet test sample is not greater than Ra 1.6; IV, the test samples are punched, the sheet test samples are put on a punching device to be punched into particle test samples with the diameter of phi 3mm to phi 10mm; V, the test samples are soaked and cleaned, the particle test samples are put into an ultrasonic soaker, newly soaked and cleaned by using acetone, and dried by hot air or natural wind. The preparation method of an element test sample in steel is simple and accurate, and can prepare the test samples in four minutes.
Description
Technical field
The preparation method of sample for determining component content in a kind of steel.
Background technology
In the fast measuring steel in the steel carbon, sulphur, nitrogen element particularly oxygen content be not only steel oxygen uptake degree quality monitoring foundation drawn in deoxidation in the steel making working procedure and continuous casting, be again to reduce inclusion content of steel, improve one of steel inherent quality key index.Traditional chemical determination oxygen content only is applicable to the liquid steel sample of aluminium deoxidation, and is not suitable for solid metal analysis oxygen content, and its method for making sample is with planer, drilling machine etc. sample to be processed into iron filings.The method for making sample that present most of solid metal is analyzed oxygen is to adopt equipment such as hollow drilling machine, lathe that sample is processed into graininess or bits sample, adopts NDIR (Non-Dispersive Infrared) absorption process instrument oxygen determination.Adopt this method sample preparation time to reach 16 minutes, can not satisfy the needs that line mass control is faced in the stokehold fully.
Summary of the invention
In order to overcome the above-mentioned deficiency of the preparation method of sample for determining component content in the existing steel, the invention provides a kind of simply, the preparation method of sample for determining component content in the steel fast and accurately.
The preparation method of sample for determining component content comprises following steps in order in this steel:
I. ladle is materialsed
With analytical cartridge with long handle, from ladle, get the sample of steel, pour out after to be cooled the solidifying, the sample that analytical cartridge is obtained is bar-shaped, the length of bar-shaped sample and diameter are convenient to clamping with cutting equipment and are advisable, long 26～the 60mm of general bar-shaped sample, the middle part diameter is 30～40mm, the tapering of bar-shaped sample is 0～0.4, (tapering be 0 o'clock be the cylinder bar) is generally two kinds of cylindrical bar and truncated cone-shaped bars, and the tapering of truncated cone-shaped bar is 0.25～0.4, (tapering be 0 o'clock be cylindrical bar), the diameter at bar-shaped sample middle part is 1/4th to 1/2nd of a length, the length of the bar-shaped sample of analytical cartridge system is in the time of guaranteeing the cutting sample, behind the thickness of each cutting of the two ends of bar-shaped sample greater than 10mm, getting the middle part is sample, and sample thickness is more than 6mm;
II. cut sample
With the bar-shaped sample of clamp clamps, bar-shaped sample is installed in cutting equipment, the cutting slice sample, the thickness of thin slice sample is not less than 6mm, and a general thin slice sample can be analyzed oxygen, carbon, sulphur and nitrogen simultaneously;
III. process thin slice sample two surfaces
The thin slice sample is put into anchor clamps, and with positive and negative two planes of plane process equipment processing thin slice sample, the value of the plane surface roughness of processing back thin slice sample is not more than R
a1.6, be generally R
a1.6-R
a0.8, during processing thin slice specimen surface, thin slice specimen surface temperature≤30 ℃, when environment temperature is higher than 30 ℃, with the liquid coolant cooling, remove the oxide layer of thin slice specimen surface in the time of processing, remove unclean as surface oxide layer, the oxygen content of being surveyed is higher, and the thickness＞1.6mm of the thin slice sample that processes is good;
IV. towards sample
The thin slice sample is placed on the particle sample that decompressor is washed into diameter of phi 3mm-Φ 10mm, is generally Φ 6mm-Φ 7mm;
V. embathe
Particle sample is put into the ultrasound wave soaker newly embathe, behind hot air dries or the natural air drying, can adopt outer chromatic dispersion infrared absorption method oxygen determination with acetone.
The preparation method of sample for determining component content is when ladle is taken a sample in the above-mentioned steel, and less than the sample of 15pmm inert gas cooling samples, general oxygen content is greater than 20pmm for oxygen content.
The preparation method of sample for determining component content is when ladle is taken a sample in the above-mentioned steel, the employing xsect is that the truncated cone-shaped tubbiness or the round barrel shape analytical cartridge of annular is preferable, the bar-shaped sample that analytical cartridge is obtained is a truncated cone-shaped or cylindrical, and the tapering of the bar-shaped sample of truncated cone-shaped is 0.25～0.4; At cutting sample configurable ring cutting clamper, the length of annular cutting clamper is the 0.3-0.6 of bar-shaped specimen length, and there is a 2mm push rod at the ring middle part, the medial surface of annular cutting clamper and the lateral surface of bar-shaped sample match, so that annular holder is clamped bar-shaped sample, take the annular cutting clamper of inboard mask for the bar-shaped sample of truncated cone-shaped with tapering, the tapering of medial surface equates with the outside tapering of the bar-shaped sample of truncated cone-shaped or adapts, (internal diameter suitable for reading that generally has the annular cutting clamper of tapering is 46-55mm, the end opening internal diameter is 32～45mm, during cutting bar-shaped sample is put into the ring specimen cutting clamper, the lower end protruded length is not less than 20mm, be convenient to processing) the ring specimen cutting clamper push rod that will press from both sides bar-shaped sample again embeds that (ring rotation when preventing to cut) annular cutting clamper is installed on the cutting equipment in the cutting trough, the setting height(from bottom) of ring specimen cutting clamper is 7.5～9.5mm, be preferably disposed on 8mm, (clamping height or length are also different because of the process equipment difference) carry out cutting operation, and cutting sample sheet thickness is not less than 6mm; When processing thin slice sample two surfaces, the thin slice sample put into to have the degree of depth be the specimen holder base of 30～50mm for the 1.2-2.0mm interior diameter, and be placed on the platform of processing plane equipment.
This method is processed into 1g left and right sides particle with sample, more satisfactory method for making sample, adopt NDIR (Non-Dispersive Infrared) absorption process instrument oxygen determination.Satisfied smelting, continuous casting working procedure oxygen quality monitoring, instruct process modification.This method also is applicable to the manufacturing to carbon, sulphur, the sample preparation of nitrogen element in the steel.This method has following advantage: A, gets block sample from steel, adopts cutting, processing sample surface, punching press only can become particle sample in 4 minutes, obviously shortens the time with other system specimen method; B: realized in the big bag, the fast measuring of oxygen on the continuous casting billet, for steel making working procedure deoxygenation of liquid steel and continuous casting draw the quality monitoring of steel oxygen uptake degree that scientific basis is provided; C, realized in the big bag, the fast measuring of oxygen on the continuous casting billet, satisfied the quality monitoring that stainless steel production process qualifying point faces line oxygen, oxygen is controlled at below the 29.06ppm in the big bag of smelting procedure stainless steel production, further improved the molten steel degree of purity, the continuous casting billet oxygen content drops to present 33.78ppm by 41ppm; D, by strengthen in the big bag of smelting procedure and the continuous casting working procedure strand improve quality the control point oxygen content face line selective examination dynamics, stainless steel moves back useless rate and reduces to 1.3% by 1.7%, a year wound is imitated 1,100,000 yuan; E, improve the analysis precision of carbon, sulphur, nitrogen element in the steel, especially improved the analysis precision of Ultra-low carbon, low-sulfur.
Description of drawings
The structural drawing of the analytical cartridge of the preparation method embodiment one of sample for determining component content in this steel of Fig. 1.
The annular of the preparation method embodiment one of sample for determining component content cutting clamping structure figure in this steel of Fig. 2.
The annular cutting clamper of the preparation method embodiment one of sample for determining component content is clamped the outside drawing of bar-shaped sample in this steel of Fig. 3.
The bar-shaped sample cutting synoptic diagram of the preparation method embodiment one of sample for determining component content in this steel of Fig. 4.
Preparation method embodiment one plane of sample for determining component content adds the clamping figure in man-hour in this steel of Fig. 5.
The preparation method embodiment's one of sample for determining component content dashes the sample synoptic diagram in this steel of Fig. 6.
Fig. 7 is the structural drawing of analytical cartridge of the preparation method embodiment two of sample for determining component content in this steel.
Fig. 8 is the outside drawing that the annular cutting clamper of the preparation method embodiment two of sample for determining component content in this steel is clamped bar-shaped sample.
Among the above-mentioned figure:
1, long handle 2, analytical cartridge 3, suitable for reading 4, go to the bottom 5, annular cutting clamper
6, suitable for reading 7, end opening 8, push rod 9, bar-shaped sample 10, cutter seam
11, thin slice sample 12, cutter seam 13, specimen holder base 14, clamping groove
15, punching 16, particle sample 17, analytical cartridge 18, suitable for reading
19, bar-shaped sample 20, annular cutting clamper 21, holding screw 22, screw
Embodiment
Describe the embodiment of preparation method of sample of the present invention in detail below in conjunction with embodiment and accompanying drawing thereof, but preparation method of sample of the present invention is not limited to following embodiment.
Embodiment one
What present embodiment prepared is 0Cr18Ni9 (GB 304) steel oxygen sample, and its step is as follows:
I. ladle is materialsed
The truncated cone-shaped tubbiness analytical cartridge 2 of the long handle 1 of apparatus, get the sample of steel from ladle, pour out after to be cooled the solidifying, the bar-shaped sample 9 that analytical cartridge 2 is obtained is the truncated cone-shaped of tapering for tool, specimen length is 40mm, end diameter of phi 48mm, top diameter are Φ 38mm, long handle 1 long 1.8m, suitable for reading 3 diameter of phi 55mm of analytical cartridge 2, go to the bottom 4 diameter of phi 35mm, high 90mm is referring to Fig. 1;
II. cut sample
Is length 26mm, 6 internal diameters suitable for reading are 46mm, end opening 7 internal diameters are that 32mm and ring middle part have the annular cutting clamper 5 of a 2mm push rod 8 to be installed on the cutting equipment, see Fig. 2, the setting height(from bottom) of annular test tapping anchor clamps 5 is 8mm, (be that cutting-height is adjusted knob to the distance between the tip position, adjust a parameter of knob for cutting equipment, the thickness of the thin slice that cuts out after the distance decision secondary cut of this place adjustment, this 8mm is for adjusting the degree of depth of knob groove) bar-shaped sample 9 is put into annular cutting clamper 5, the lower end protruded length is 25mm, annular cutting clamper 5 push rods 8 with the bar-shaped sample 9 of clamping embed in the groove of cutting equipment again, carry out cutting operation, cutting sample sheet thickness is 6.2mm, sees Fig. 3 and Fig. 4;
III. process thin slice sample two surfaces
IV. towards sample
V. embathe
VI. oxygen determination
With the TC500 type oxygen nitrogen instrument that particle sample 16 usefulness U.S. Leco Corporations produce, adopting the NDIR (Non-Dispersive Infrared) absorption process to record oxygen content is 0.4ppm-0.2%.
The used cutting equipment of present embodiment is the VST-2S cutting machine that German He Zuoge produces, and processing plane equipment is the HS-FF milling machine that German He Zuoge produces, and pressing equipment is the HUST puncher.Analytical instrument is a U.S. Leco Corporation oxygen nitrogen instrument: the TC500 type.
Embodiment two
What present embodiment prepared is AISI304 (for U.S. mark 304) steel carbon sample, what use when ladle is taken a sample is drum conformal analysis sampler 17, see that the bar-shaped sample 19 that Fig. 7 analytical cartridge 17 is obtained is cylindrical, see Fig. 8, specimen length is 50mm, diameter of phi 36mm, when cutting bar-shaped sample 19, with annular cutting clamper 20, during processing thin slice sample two surfaces, roughness is R
a0.8 other step is identical with embodiment one with device therefor.Recording carbon content is 0.4ppm-6.0%.
Embodiment three
What present embodiment prepared is SUS304 (this steel grade is a day mark 304) steel sulphur sample, what use when ladle is taken a sample is drum conformal analysis sampler 17, the bar-shaped sample 19 that analytical cartridge 17 is obtained is for cylindrical, specimen length is 48mm, diameter of phi 36mm, when cutting bar-shaped sample 19, directly clamp bar-shaped sample 19 by the lathe tool cutting with lathe, other step is identical with embodiment one with device therefor.Recording sulfur content is 0-0.4%.
Embodiment four
What present embodiment prepared is 1Cr18Ni9Ti steel nitrogen sample, and its step is identical with embodiment one with device therefor.Recording nitrogen content is 0.4ppm-3.0%.
Also available common horizontal milling machine of equipment or lathe that above-mentioned four present embodiments are used, also available common vertical milling machine of processing plane equipment or grinding machine, the also available common punch press of pressing equipment.
The also available thin slice sample of above-mentioned four embodiment is analyzed oxygen, carbon, sulphur and nitrogen respectively.With the CS-600 analyser of leco company, use the TC-500 analyser of leco company when analyzing N and O when analyzing C and S
Claims (2)
1, the preparation method of sample for determining component content in a kind of steel, described preparation method comprises following steps in order:
I. ladle is materialsed
With analytical cartridge with long handle, from ladle, get the sample of steel, pour out after to be cooled the solidifying, the sample that analytical cartridge is obtained is bar-shaped, the length of bar-shaped sample and diameter are convenient to clamping with cutting equipment and are advisable, the tapering of bar-shaped sample is 0～0.4, the diameter at bar-shaped sample middle part is 1/4th to 1/2nd of a length, the length of the bar-shaped sample of analytical cartridge system, in the time of guaranteeing the cutting sample, behind the thickness of each cutting of the two ends of bar-shaped sample greater than 10mm, getting the middle part is sample, and sample thickness is more than 6mm;
II. cut sample
With the bar-shaped sample of clamp clamps, bar-shaped sample is installed in cutting equipment, the cutting slice sample, the thickness of thin slice sample is not less than 6mm;
III. process thin slice sample two surfaces
The thin slice sample is put into anchor clamps, and with positive and negative two planes of plane process equipment processing thin slice sample, the value of the plane surface roughness of processing back thin slice sample is not more than R
a1.6, during processing thin slice specimen surface, thin slice specimen surface temperature≤30 ℃, the oxide layer of removal thin slice specimen surface in the time of processing;
IV. towards sample
The thin slice sample is placed on the particle sample that decompressor is washed into diameter of phi 3mm-Φ 10mm;
V. embathe
Particle sample is put into the ultrasound wave soaker newly embathe, hot air dries or natural air drying with acetone.
2, the preparation method of sample for determining component content in the steel according to claim 1 is characterized in that: when the I. ladle was materialsed, the sample that analytical cartridge is obtained was the bar-shaped sample of truncated cone-shaped, and the tapering of the bar-shaped sample of truncated cone-shaped is 0.25～0.4; When III. processing thin slice sample two surfaces, the value of the plane surface roughness of processing back thin slice sample is R
a1.6-R
a0.8.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100129268A CN100451602C (en) | 2006-07-06 | 2006-07-06 | Preparation method of steel sample for determining component content in steel |
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| CNB2006100129268A CN100451602C (en) | 2006-07-06 | 2006-07-06 | Preparation method of steel sample for determining component content in steel |
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| CN1884995A CN1884995A (en) | 2006-12-27 |
| CN100451602C true CN100451602C (en) | 2009-01-14 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101078673B (en) * | 2007-07-06 | 2010-06-16 | 河北钢铁股份有限公司 | Converter terminal gas all-analysis sampling method by determining carbon-oxygen equilibrium |
| CN102564952A (en) * | 2010-12-07 | 2012-07-11 | 苏州春兴精工股份有限公司 | Simple testing device for spectrum sample block |
| CN103837364B (en) * | 2012-11-20 | 2015-12-09 | 江苏天工钛业科技有限公司 | A kind of titanium material sampler |
| CN110967236A (en) * | 2019-12-19 | 2020-04-07 | 中国航发哈尔滨轴承有限公司 | Preparation method of sample for measuring oxygen content in G13Cr4Mo4Ni4V steel |
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| JPH0331739A (en) * | 1989-06-29 | 1991-02-12 | Aichi Steel Works Ltd | Chemical analysis of metallic material |
| CN2259624Y (en) * | 1995-10-19 | 1997-08-13 | 上海第三钢铁厂 | Sampling device for detecting molten steel in steel ladle |
| CN1177100A (en) * | 1996-09-19 | 1998-03-25 | 日本钢管株式会社 | Method and equipment for analysing solid samples |
| CN1060270C (en) * | 1995-08-22 | 2001-01-03 | 杭州钢铁集团公司 | Quick iron and steel component response technique for steel smelting platform |
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2006
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0331739A (en) * | 1989-06-29 | 1991-02-12 | Aichi Steel Works Ltd | Chemical analysis of metallic material |
| CN1060270C (en) * | 1995-08-22 | 2001-01-03 | 杭州钢铁集团公司 | Quick iron and steel component response technique for steel smelting platform |
| CN2259624Y (en) * | 1995-10-19 | 1997-08-13 | 上海第三钢铁厂 | Sampling device for detecting molten steel in steel ladle |
| CN1177100A (en) * | 1996-09-19 | 1998-03-25 | 日本钢管株式会社 | Method and equipment for analysing solid samples |
| CN2432573Y (en) * | 2000-07-25 | 2001-05-30 | 宝山钢铁股份有限公司 | Molten steel sampling cup |
Non-Patent Citations (2)
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| 转炉钢熔炼化学成分取样方法探讨. 冯跃平等.新疆钢铁，第1期. 2004 |
| 转炉钢熔炼化学成分取样方法探讨. 冯跃平等.新疆钢铁，第1期. 2004 * |
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Owner name: SHANXI TAIGANG STAINLESS STEEL CO., LTD. Free format text: FORMER OWNER: TAIYUAN IRON AND STEEL (GROUP) CO LTD Effective date: 20070629 |
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