CN100585380C - Production method of high-homogeneity chromium-nickel austenite stainless steel optical spectrum calibration example - Google Patents
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Abstract
The present invention discloses a method for preparing the high-homogeneity chromium-nickel austenite stainless steel optical spectrum correcting sample in order to provide a reliable optical spectrum correcting sample. The method comprises the following steps: 1) correcting the component of the sample to the following mass percentage: C<=0.20, Si<=1.0, Mn<=2.0, P<=0.035, S<=0.030, Cr 16-24, Ni 6-14, and the rest is Fe; 2) smelting and casting to steel ingot with the components; 3) smithing with the staring temperature: 1100 DEG C-1150 DEG C, and the finishing temperature: 900 DEG C-950 DEG C; 4) roller milling with staring temperature: 1100 DEG C-1150 DEG C, and the finishing temperature: 900 DEG C-950 DEG C; and 5) heat treating for solution temperature 1000 DEG C-1050 DEG C and temperature preserving time 40-50min, and at last water cooling with immersion type. The invention corrects the homogeneous austenite structure with grain fineness number larger than 7 and residual ferrite dispersed arranged in the sample block, satisfies the request of the spectrum analysis and leads to that the spectrometry obtains the best analyzing precision.
Description
Technical field
The present invention relates to steelmaking process composition control analysis technical field, particularly chromiumnickel austenite stainless steel steelmaking process composition control analysis technology.
Background technology
Austenitic stainless steel is a most important steel class in the stainless steel, and its turnout and use amount account for 70% of stainless steel total production and consumption.According to keeping the alloying mode that the alloy austenite matrix is taked, austenitic stainless steel can be divided into chromium nickel stainless steel and chromium manganese stainless steel two big series.Wherein, chromiumnickel austenite stainless steel main chemical scope commonly used is as shown in table 1:
Table 1 is used chromiumnickel austenite stainless steel chemical analysis scope, wt% always
| Element | C | Si | Mn | P | S | Cr | Ni |
| The composition scope | ≤0.20 | ≤1.0 | ≤2.0 | ≤0.035 | ≤0.030 | 16～24 | 6～14 |
At present, in the chromiumnickel austenite stainless steel production run, in order to reduce cost and to guarantee that production run is smooth and easy, the control accuracy of the contour alloying element of Ni requires more and more higher.Though analyze at Ni, the higher X-fluorescence analysis means of precision are arranged, owing to the factors such as restriction of rhythm of production to analysis time, the spark source emission spectrum that each element is measured is simultaneously still born main analysis task.Accuracy in analytical accuracy and the selected standard sample for spectrochemical analysis fiducial interval is consistent.For reaching the accuracy target of spark source emission spectrum the best, should adopt corresponding (similar) spectrum correction sample to make type and proofread and correct to the testing sample matrix.Therefore, it is good to make analysis precision, and the good high uniformity spectrum correction sample of accuracy is necessary then.
Usually adopt in identical steel grade production scene with die casting sampling, definite value voluntarily, as correcting sample in traditional manual laboratory.The correcting sample of this as cast condition has been successfully applied to each steel mill.But just not too suitable for large-scale full-automatic laboratory, major defect is: monolithic is made, size is irregular, the definite value workload big, the definite value error is uncertain and do not meet the laboratory certification standard.Therefore, the forging attitude of specialization making in enormous quantities at present has the development of card spectrum correction sample very rapid.In fact, in general, fields such as low alloy steel, carbon steel do not find the serious bad phenomenon of standard specimen homogeneity as yet, thereby this type of has card spectrum correction sample to obtain good application in the large automatic laboratory such as Baogang Stocks Trading Co.'s Baosteel Branch's at home.But,, but run into the bad problem of homogeneity for the Cr that card is arranged, Ni austenite stainless steel optical spectrum standard specimen.
Domestic chromium-nickel austenite stainless steel optical spectrum correcting sample generally adopts ingot casting through forging, hot rolling (1150 ℃～1260 ℃ of conventional start rolling temperatures, about 800 ℃ of finishing temperatures), all steps such as inspection, definite value preparations, with general carbon steel, in, no significant difference such as low alloy steel, and it be purpose that forging, hot rolling are only handled with " be shaped and make the densification of sample block structure ", considers the influence of tissue to the chromium-nickel austenite stainless steel optical spectrum analysis as yet.
From the metallographic microstructure of the material object of external professional standard specimen company as can be seen, its chromium-nickel austenite stainless steel optical spectrum standard specimen has all passed through solution treatment, but the degree of solution treatment is very inconsistent, and individual other style piece exists visibly different structural state on the cross section of diameter 38mm.This solution treatment effect should be that water quenching forms after the hot rolling, is not the solution treatment that has purpose specially to carry out; And in manufacture process, do not control the grain size of sample piece yet.
Organize and unreasonablely may cause that it is spectrum worker's common recognition that the spectral analysis precision worsens, but that studies comparative maturity at present mainly is confined to the pig iron, cast iron air chill problem, and having formed its special standard sample for spectrochemical analysis technology of preparing, the unreasonable precision that causes spectral analysis Ni is bad does not appear in the newspapers as yet and the austenite stainless steel optical spectrum standard specimen is organized.
Have this unevenness phenomenon of card chromium-nickel austenite stainless steel optical spectrum standard specimen not obtain as yet paying attention to, its reason can be summarized as follows:
1, the emission spectrum technology is greatly improved in recent years at the precision level of high-load section.To factor---the excitation source that the whole instrument precision has the greatest impact, the appearance owing to digital light has had significant progress.The Evaluation for Uniformity of standard model is directly related with assay method or instrument level, and the inhomogeneous of sample is absolute, evenly is relative.The homogeneity of so-called sample comes down to the degree of irregularity of sample with respect to the measurement stochastic error of used measuring method or the result who draws for the re-set target of characteristic value uncertainty.The emission spectrographic analysis development of technology, and more and more higher precision control requires just to make this unevenness phenomenon come out to the contour alloying element of Ni in producing in recent years.
2, the chromium-nickel austenite stainless steel optical spectrum correcting sample that forges attitude is not used widely as yet, and the user knows from experience not dark to this unevenness phenomenon.General spectral standard sample only is applied to the drafting of working curve, and the most of steel mill of the actual correcting sample that uses still adopts self-control as cast condition sample, most of user does not further investigate forging attitude, having this homogeneity condition of poor cognition of card correcting sample not dark yet.
Prior art is not considered the influence of chromiumnickel austenite stainless steel tissue to the spectral analysis result as yet, does not more take corresponding means that it is controlled in manufacturing process.This spectrum sample piece that does not obtain by uniform formation's deformation and abundant solid solution, its tissue morphology is very undesirable: sample interblock (even in sample piece) grain size does not wait from 5.0～8.5 grades; A little ferrite local accumulation in the sample piece, skewness.For spectrometer analysis, it is bad to show as homogeneity.
The grain size of chromiumnickel austenite stainless steel inhomogeneous mainly forge, distortion inhomogeneous causing, particularly chromiumnickel austenite stainless steel have the characteristics of anti-strong adaptability in the operation of rolling, easilier cause that distortion is inhomogeneous.Grain size is inconsistent, and structure stability is inconsistent, also may be interpreted as the potential energy difference of tissue, influenced spectrum evaporation, process such as excite.Thereby influenced the mensuration precision of nickel.
Because the requirement of spectral analysis itself, the composition of spectrum correction sample should be close with testing sample matrix composition.And the stainless steel kind is because the requirement of combination property, and the Cr/Ni of specification composition is than under the condition, the inevitable ferrite that easily produces a few percent.And ferrite and austenite there are differences in composition composition, evaporation energy, excitation energy etc.So the ferrite skewness also directly influences the precision of Ni spectral analysis in the chromiumnickel austenite stainless steel standard specimen.
Because ferrite mainly is to distribute along austenite grain boundary, so the refinement of austenite crystal is to ferritic disperse decisive role.And solution treatment can make the austenite structure homogenising on the one hand, ferrite is reduced or disappearance, and residual ferrite more disperse is distributed in the sample piece.
Therefore, think after a large amount of chromium nickel standard sample microstructures and the spectrum Ni analysis precision both at home and abroad in comparison research: the bad phenomenon of chromium-nickel austenite stainless steel optical spectrum standard specimen homogeneity can reduce factor aspect the following microstructure: one) grain size inhomogeneous in the sample piece.Two) the ferritic skewness that may exist.A little ferrite in the chromiumnickel austenite stainless steel is grown along austenite grain boundary, presents local accumulation, phenomenon pockety.
Comparative Examples 1, domestic former Shanghai steel grind YSBS20310-3-2006Cr, Ni austenitic stainless steel 304 (the SUS trade mark) spectrum correction sample the time find, with the measurement standard deviation S of lot number standard model spectral analysis Ni 0.03～0.10% (seriously inhomogeneous in the piece).Randomly draw 8 samples, concrete measurement data sees Table 2.
Table 2 spectrum correction sample YSBS20310-3-2006 nickel element measurement standard deviation
Comparative Examples 2, the YSBS15325-20050Cr18Ni9 chromium-nickel austenite stainless steel optical spectrum standard model of Taiyuan Iron ﹠ Steel's development in 2005, all inspection data in its spectrum development report see Table 3.
Table 3 Taiyuan Iron and Steel Co. variance method uniformity testing (Ni) raw data
Data presentation goes out seriously inhomogeneous in its piece (the maximum extreme difference of measured value is 0.37%).Though by adopting variance method to carry out the uniformity testing result is qualified, owing to exist the variation of the interior variation of significant piece statistically greater than measuring method, thereby in fact this sample can not be judged as evenly.，
Comparative Examples 3, external professional standard specimen company such as U.S. Brammer Standard Company, the interior homogeneity of the piece of Ni is also very inconsistent in the standard specimen of different trade mark chromiumnickel austenite stainless steels such as Inc., Analytical Reference Materials International.The measurement standard deviation is 0.031～0.150%.
Test data sees Table 4:
Table 4 U.S. standard specimen company austenitic stainless steel standard model nickel element measurement standard deviation
But when being analyzed Ni, the spectral standard sample random sampling wet chemical of above-mentioned Comparative Examples 1,2 finds that its composition is almost completely consistent.So forging the interior homogeneity of attitude chromium-nickel austenite stainless steel optical spectrum correcting sample standard sample for spectrochemical analysis piece relatively poor is that above-mentioned standard model is organized the unreasonable result who influences the spark source emission spectrographic analysis.Lack of homogeneity has had a strong impact on the validity of correction and the control of routine analysis precision.Once attempt to adopt method for screening select homogeneity preferably sample be used for daily correction, but since in the piece depth direction exist inhomogeneously equally, still can't satisfy the requirement of routine analysis.
Existing technology is:
1) forges, to be shaped, to make the densification of sample piece is purpose, applies mechanically the big technology of producing of industry, does not pass through autotelic optimization: adopt routine to open and forge 1150 ℃～1260 ℃ of temperature, about 800 ℃ of final forging temperatures, the grain size size and the homogeneity of ultimate criterion sample piece there is not technical requirement;
2) rolling, there is not specially requirement, with further shaping, to make the densification of sample piece be purpose, applies mechanically the big technology of producing of industry, do not pass through autotelic optimization: adopt routine to open and forge 1150 ℃～1260 ℃ of temperature, about 800 ℃ of final forging temperatures.
3) solution treatment, it is indeterminate not have this process procedure or target, and technology is unreasonable.
Because above-mentioned forging and the unreasonable crystal grain that causes of rolling sequence technology is thick and inhomogeneous can't the improvement by thermal treatment, this is that the characteristic of chromiumnickel austenite stainless steel determines.Cause sample piece grain size not wait ferrite local accumulation, skewness from 5.0～8.5 grades.For spectrometer analysis, it is bad to show as homogeneity.
Summary of the invention
The object of the present invention is to provide a kind of high-homogeneity chromium-nickel austenite stainless steel optical spectrum emendation example and preparation method thereof, the structural state of desirable spectrum correction sample is proposed, guarantee the tissue that reaches desirable, thereby eliminate this influence of organizing irrationality to spectral analysis substantially, for the laboratory provides reliable spectrum correction sample or as statistical Process Control (SPC) sample.
The present invention proposes: for the chromium-nickel austenite stainless steel optical spectrum correcting sample, residual ferrite is disperse and distributes, and in the piece grain size greater than 7 grades, the austenite structure state is the most rational tissue morphology uniformly.And by even fully deformation and fully solid solution just can obtain the spectrum sample piece of this tissue morphology.
The present invention points out the homogeneity of chromium-nickel austenite stainless steel optical spectrum standard specimen, and not only the homogeneity with its chemical analysis is relevant, and closely related with the rationality of organization of standard sample for spectrochemical analysis; Need to use corresponding means in preparation process, crystal grain thinning to 7.5～8.0 grade simultaneously by sufficient solution treatment, are controlled remaining ferritic amount and distribution, thereby are prepared spectrometer, show as the qualified samples of high uniformity.
For achieving the above object, technical scheme of the present invention is,
The preparation method of high-homogeneity chromium-nickel austenite stainless steel optical spectrum emendation example, it comprises the steps:
1) the composition quality number percent of correcting sample is: C≤0.20, Si≤1.0, Mn≤2.0, P≤0.035, S≤0.030, Cr16～24, Ni 6～14, surplus are iron;
2) smelt, be cast as steel ingot by mentioned component;
3) forge, open the forging temperature: 1100 ℃～1150 ℃, final forging temperature: 900 ℃～950 ℃, multi-faceted forging under the situation of steel ingot internal and external temperature unanimity, jumping-up pulling repeatedly makes its homogeneous deformation, be shaped with the basis that makes the densification of sample piece on reach crystal grain thinning, the consistent purpose of tissue;
4) rolling, start rolling temperature: 1100 ℃～1150 ℃, finishing temperature: 900 ℃～950 ℃; Further evenly, crystal grain thinning;
5) thermal treatment, 1000 ℃～1050 ℃ of solid solubility temperatures, temperature retention time 40～50min, the immersion water-cooled reaches both fully solid solutions, the effect of avoiding austenite crystal to grow up again simultaneously then.
The correcting sample destination organization is 7～7.5 grades at center, 7.5～8 grades uniform formation on every side.
Grain size is the uniform austenite structure that disperse distributes greater than 7 grades, residual ferrite in the correcting sample piece of the present invention.For spectrometer analysis, show as high uniformity.
The spark source emission spectrum should adopt matrix similar in order to reach best mensuration precision, and the correcting sample that composition is close is made type and proofreaied and correct.The internal control target that modern stainless steel is produced Ni is about 0.20% close limit, and produces greatly and adopt the technology of progressively adjusting to the right place, suits to adopt in the spark source emission spectrographic analysis control device of correcting sample as composition especially.The spectrum correction sample of high uniformity can improve the accuracy of this correction.Generally speaking, the fiducial interval of corrected value is directly related with the homogeneity of spectrum correction, with formulate is
Standard deviation desired value S＜0.03%.
The mensuration precision that experiment shows chromium, austenitic standard model is closely related with organizing of sample itself, so the preparation process of high uniformity chromium, austenitic standard model must strictness be controlled corresponding technological parameter.
Under the condition of ratio of compression basic fixed,, help crystal grain thinning in chromium, the suitable low side operation of forging, rolling temperature province of austenitic stainless steel.Adopt repeatedly forge, rolling, pier slightly pulls out repeatedly, the amount of the each distortion of control helps even crystal grain thinning.And reasonably solution treatment distributes ferritic disperse, and avoids the irrational of grain size to grow up.The crystal grain that above-mentioned forging and rolling sequence technology irrationality cause thick and inhomogeneous be irreversible, can't improve by thermal treatment, therefore must strict control.
The invention has the beneficial effects as follows,
By the standard model that method of the present invention is made, not only guaranteed the even of chemical constitution, also guaranteed the uniformity of tissue.In the application of spectral analysis, each by the excitation of spectra that several thousand sparks are formed, is avoided irrational result's of being caused by sample itself generation, make spectroscopic assay obtain best analysis precision.Use correcting sample of the present invention, can significantly improve chromiumnickel austenite stainless steel steelmaking process composition control analysis precision, ensure the realization of actual chromium nickel composition working control precision target in the chromiumnickel austenite stainless steel production, reduce the unnecessary expensive metal consumption, thereby produce huge economic benefit.
The present invention is applicable to the spark source emission spectrographic analysis, is particularly suitable for large automatic laboratory and adopts.
Embodiment
Embodiment 1
Select for use the high-quality continuous casting billet of corresponding steel grade to make masterbatch, adopt the 1000Kg intermediate frequency furnace to smelt, guaranteeing the homogeneity of chemical analysis, and finely tune composition by the requirement of correcting sample.
Pour into φ 360mm/300mm billet, behind ingot casting excision head (25～30%), the tail (15～20%), peeling is handled, and portion exists the loose tissue defects that waits to excise end to end.
Ingot casting forges: select to open 1100 ℃～1150 ℃ of temperature of forging, 900 ℃～950 ℃ of final forging temperatures; Guarantee steel ingot internal and external temperature unanimity, strictness rapid, multi-faceted (six faces) in the control temperature evenly forges; Jumping-up pulling repeatedly divides the square billet that forges into 76mm * 76mm * 100mm for four times.
Billet rolling: select 1100 ℃～1150 ℃ of start rolling temperatures, 900 ℃～950 ℃ of finishing temperatures,, be rolled into Φ 40mm round steel with the square billet of 76mm * 76mm * 100mm.
Select 1000 ℃～1050 ℃ of solid solubility temperatures, temperature retention time 45min, the immersion chilling.Reach both fully solid solutions, the effect of avoiding austenite crystal to grow up again simultaneously.Destination organization is 7～7.5 grades at center, 7.5～8 grades uniform formation on every side.
Other embodiment are referring to table 5, according to technical scheme of the present invention, with the trade mark (301,304,309S) difference, preparation chromium-nickel austenite spectrum correction standard specimen.
Table 5
In sum, the present invention is by evenly fully deformation and fully solid solution, making in the tissue morphology of spectrum sample piece residual ferrite be disperse distributes, and grain size is greater than 7 grades, uniform austenite structure state in the piece, satisfy the requirement of spectral analysis, make spectroscopic assay obtain best analysis precision, can significantly improve chromiumnickel austenite stainless steel steelmaking process composition control analysis precision, ensure the realization of actual chromium nickel composition working control precision target in the chromiumnickel austenite stainless steel production, reduce the unnecessary expensive metal consumption, thereby produce huge economic benefit.
Claims (1)
1. the preparation method of high-homogeneity chromium-nickel austenite stainless steel optical spectrum emendation example, it comprises the steps:
1) the composition quality number percent of correcting sample is: C≤0.20, Si≤1.0, Mn≤2.0, P≤0.035, S≤0.030, Cr16～24, Ni 6～14, surplus are iron;
2) smelt, be cast as steel ingot by mentioned component;
3) forge, open the forging temperature: 1100 ℃～1150 ℃, final forging temperature: 900 ℃～950 ℃, multi-faceted forging, jumping-up pulling repeatedly makes its homogeneous deformation;
4) rolling, start rolling temperature: 1100 ℃～1150 ℃, finishing temperature: 900 ℃～950 ℃;
5) thermal treatment, 1000 ℃～1050 ℃ of solid solubility temperatures, temperature retention time 40～50min, immersion water-cooled then;
6) obtaining the correcting sample destination organization is 7～7.5 grades at center, and 7.5～8 grades on every side, residual ferrite is the uniform austenite structure that disperse distributes.
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| CN102051531B (en) * | 2009-10-27 | 2012-11-14 | 宝山钢铁股份有限公司 | High boron content austenite stainless steel and preparation method thereof |
| CN102284685B (en) * | 2010-06-18 | 2013-04-10 | 中国科学院金属研究所 | Method for anatomical inspection on quality, structure and performance of steel ingot of 70-ton grade to 600-ton grade |
| CN102126121B (en) * | 2010-12-08 | 2013-02-27 | 扬州诚德重工有限公司 | New process combining forging and rolling |
| CN102605285B (en) * | 2011-01-25 | 2014-05-07 | 宝山钢铁股份有限公司 | Austenitic stainless steel and method for manufacturing same |
| CN102230137A (en) * | 2011-06-20 | 2011-11-02 | 宣达实业集团有限公司 | Austenitic heat-resistant stainless steel and processing method thereof |
| CN102313661B (en) * | 2011-07-28 | 2013-06-12 | 山西太钢不锈钢股份有限公司 | Preparation method of stainless steel 304, TB 310 standard spectrum sample |
| CN102989819A (en) * | 2012-12-11 | 2013-03-27 | 江苏永钢集团有限公司 | Steel production process with forging-rolling combination |
| CN105021534B (en) * | 2015-07-21 | 2017-07-18 | 河北钢铁股份有限公司邯郸分公司 | A kind of method of detection 20CrMnTi structure of steel composition and content |
| CN106077379B (en) * | 2016-06-20 | 2019-09-27 | 安徽省瑞杰锻造有限责任公司 | A kind of forging technology of 0Cr23Ni13 heat-resistance stainless steel |
| CN109596531B (en) * | 2018-10-29 | 2021-09-28 | 酒泉钢铁(集团)有限责任公司 | Preparation method of ultra-pure ferrite stainless steel spectrum standard sample |
| CN112662935A (en) * | 2020-12-07 | 2021-04-16 | 中兴能源装备有限公司 | Control method for ferrite content of nitrogen-controlled austenitic stainless steel forging |
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