CN102486442A - Preparation method of ultra-low-carbon steel standard substance, and corresponding ultra low carbon determination method - Google Patents
Preparation method of ultra-low-carbon steel standard substance, and corresponding ultra low carbon determination method Download PDFInfo
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- CN102486442A CN102486442A CN2010105739079A CN201010573907A CN102486442A CN 102486442 A CN102486442 A CN 102486442A CN 2010105739079 A CN2010105739079 A CN 2010105739079A CN 201010573907 A CN201010573907 A CN 201010573907A CN 102486442 A CN102486442 A CN 102486442A
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Abstract
The invention relates to a standard substance used in content determination of carbon in steel, and a corresponding determination method. The preparation method of the ultra-low-carbon steel standard substance comprises steps that: (1) according to an ultra low carbon content range requirement, within a content range of 0.0005-0.005%, a certain content gradient is designed; smelting, ingot casting or factory on-site sampling is carried out, such that a billet is obtained; the billet is processed through decorticating and forging, such that a bar is obtained; (2) the bar is turned into sample particles or sheets, and a particle number per gram is controlled at 200-600; during the processing procedure, overheating should be prevented, and the sample should not be grinded; (3) the machined sample is subject to zinc or nickel plating; (4) the sample is sealed by using a glass or plastic bottle with an inner cap, or is packaged by an additional sealing card box, such that a ten-year quality guarantee period commonly required by standard substances is ensured. Carbon contents of a production sample and the standard substance are determined by using a common method. With the method provided by the invention, 5 to 10 minutes of preheating is not required, such that an actual analysis speed satisfy a requirement of a production technology.
Description
Technical field
The present invention relates to the mensuration of carbon content in the steel, relate in particular to determination of carbon content is used in a kind of steel standard substance and corresponding assay method.
Background technology
Ultralow-carbon is measured and to be referred generally in the steel to refer in particular to the mensuration of the carbon of 5-50ppm scope in the steel less than the mensuration of 0.01% carbon in the steel.Ultralow-carbon mensuration generally, also is mainly to adopt infrared absorption determining at present in the steel, and Ultra-low carbon standard substance in the steel is adopted in the correction of instrument.
The standard GB of carbon infrared analysis method/T 20126-2006 in the steel " the mensuration second portion of non-alloy steel low carbon content: infrared absorption method after induction furnace (through the preheating) internal combustion " and GB/T20123-2006 " the mensuration Efco-Northrup furnace burning back infrared absorption method (conventional method) of the total carbon and sulphur contents of iron and steel "; Corresponding international standard ISO15349 of adopting by equivalent and ISO15350 are the representative or the carrier of Ultra-low carbon determination techniques in the existing steel.
In the GB/T 20126-2006 method standard, before measuring, sample needs, so be called for short preheating method, measurement range 0.0003-0.010% at 420 ℃ of muffle furnace thermal pretreatment 5-10min; In GB/T 20123 method standards, sample need not thermal pretreatment before measuring, so be called for short conventional method, measurement range 0.005-4.3%.
The conventional method regulation is measured and is limited to 0.005% down mainly is the interference of considering that specimen surface carbon is measured Ultra-low carbon in the steel; Specimen surface carbon exists by infrared absorption swarming method experiment institute real example; Specimen surface carbon influences the accuracy that the Ultra-low carbon conventional method is measured, so lower limit can only be decided to be 0.005%.Preheating method has been eliminated the interference that surface carbon is measured Ultra-low carbon in the steel, being improved of accuracy, but the measure of preheating 5-10min before measuring makes the actual analysis speed receive too big influence.The contradiction of reality is: the preheating method accuracy can be satisfied the requirement of ultra-low-carbon steel smelting process control, but speed does not satisfy; Conventional method speed can satisfy the requirement of ultra-low-carbon steel smelting process control, but accuracy is not satisfied.
It is generally acknowledged that specimen surface carbon is absorption carbon; Previous research simultaneously reckons without the production sample to be measured (hereinafter to be referred as production appearance to be measured) of from bulk sample, producing the back and directly measuring and constitutes different phenomenons with standard substance specimen surface carbon; Production appearance to be measured must be done identical preheating pre-treatment with standard substance, so that the actual analysis speed of preheating method can not satisfy the requirement of ultra-low-carbon steel production technology.
According to the viewpoint of absorption carbon, in sample preheating-cooling procedure, surface carbon has experienced desorb--adsorption process again, can expect that the determination of carbon content value before and after the sample preheating cooling processing is consistent.
Yet the metal erosion theory is thought: iron is can " not get rusty " in water-less environment, and iron planar water in atmosphere forms surperficial moisture film, and oxygen and carbon dioxide is dissolved in behind the specimen surface moisture film and iron chemical combination; Also there is small amount of carbonate in the Main Ingredients and Appearance of iron rust except that iron oxide.In the atmosphere, the corrosion process of carbon dioxide to sample in specimen surface oxidation, association, thereby steel Ultra-low carbon conventional method is measured the generation appreciable impact.Be different from production appearance to be measured, standard substance sample long period in preparation, keeping and use is exposed to atmosphere, has surface oxidation in various degree, and its surface carbon also contains copmbined-carbon.Obviously be not enough to explain the difference of Ultra-low carbon standard substance surface carbon in production sample to be measured and the steel with the viewpoint of absorption carbon.And, fact proved, when the preparation infrared absorption determining is used sample from bulk sample; During the thermal oxide of the serious mistake of sample, the conventional method measured value is higher, this shows; Existing conventional method assay method fails to consider the influence of copmbined-carbon, this precision of influence mensuration greatly.
Summary of the invention
The present invention is intended to address the above problem, and a kind of preparation method and corresponding Ultra-low carbon assay method of ultra-low-carbon steel standard substance is provided.The present invention is the technology of preparing of Ultra-low carbon standard substance in a kind of steel that does not contain surperficial copmbined-carbon; Use Ultra-low carbon standard substance in the steel of method of the present invention preparation; Carry out ultralow-carbon mensuration in the daily steel, do not need preheating 5-10min, thereby make its actual analysis speed satisfy manufacturing technique requirent.
A kind of preparation method of ultra-low-carbon steel standard substance, it comprises the following steps:
1) according to the requirement of Ultra-low carbon content range, in the 0.0005-0.005% content range, design certain concentration gradients, base is got at smelting, ingot casting or factory scene, removes the peel, forges rod appearance;
2) turning is processed into granular or the sheet sample, controls every gram granule number at 200-600, and that process need prevent is overheated, must not grind sample;
3) the zinc-plated or nickel with the sample after the car system;
4) glass of employing band inner cap, plastic bottle encapsulate or join sealed paper box package sample in addition, to guarantee the general 10 year shelf-life that requires of standard substance.
Described ultra-low-carbon steel standard substance is measured corresponding Ultra-low carbon content method, production appearance to be measured and standard substance, is moved to and is cooled to room temperature in the exsiccator after 10 minutes in 420 ℃ of thermal pretreatment jointly, and in 48 hours, adopt conventional method to measure its carbon content.
The present invention will influence the specimen surface carbon that Ultra-low carbon infrared absorption conventional method is measured in the steel and further be divided into absorption carbon and copmbined-carbon.Produce the production specimen surface absorption carbon to be measured that the back is directly measured from bulk sample; The standard substance surface also contains copmbined-carbon except that containing absorption carbon.Because standard substance and production appearance to be measured all contain a small amount of absorption carbon that equates, influencing the principal element that Ultra-low carbon is measured in the steel is the copmbined-carbon that standard substance changes.
Though the influence that the specimen surface oxidation is measured oxygen in the influence unmatchful steel far away of Ultra-low carbon mensuration in the steel is responsive, but still have a strong impact on ultralow-carbon conventional method mensuration in the steel.Be similar to the mensuration of oxygen in the steel, produce the production appearance that the back is directly measured, can think that there is not copmbined-carbon in its surface, thereby can improve conventional method, make ultralow-carbon mensuration in its suitable steel from bulk sample.
Ultra-low carbon standard substance surface does not contain copmbined-carbon in the steel of the present invention's preparation,, coupling consistent with the production sample of behind the shape specimen preparation, directly measuring.Use Ultra-low carbon standard substance in the steel of method of the present invention preparation; The Ultra-low carbon of the daily production sample of directly measuring from bulk sample preparation back is measured; Standard substance and production sample to be measured all need not at 420 ℃ of muffle furnace thermal pretreatment 5-10min, and measured value is consistent with preheating method.Ultralow-carbon is measured program, the flow process that can use conventional method in the steel, has reduced determination step, and key is the thermal pretreatment time of having practiced thrift 5-10min, is very significant in the technology controlling and process of ultra-low-carbon steel production.In addition; Ultra-low carbon standard substance according to the preparation of present patent application technology does not contain copmbined-carbon; Homogeneity depends primarily on the homogeneity of base material in conventional method is measured; And the homogeneity of base material be prone to guaranteed, so prepared according to the methods of the invention Ultra-low carbon standard substance homogeneity in conventional method is measured does not contain the good of coating than general.
Embodiment
The principal element that influences Ultra-low carbon conventional method accuracy of measurement in the steel is the instability and the unevenness of Ultra-low carbon standard substance surface copmbined-carbon.Add oxygen standard substance preparation decades in the steel of coating, use experience proof coating is effectively to weather-resistant, can satisfy the requirement of standard substance stability.Add that Ultra-low carbon standard substance surface does not contain chemical carbon in the steel of coating;, coupling consistent with the production sample to be measured of producing the direct mensuration in back from bulk sample, the infrared absorption determining of production sample to be measured can be by GB/T20123-2006 " the mensuration Efco-Northrup furnace burning back infrared absorption method (conventional method) of the total carbon and sulphur contents of iron and steel " flow process expansion.Detailed technical scheme is as follows: a kind of preparation method of ultra-low-carbon steel standard substance, it comprises the following steps:
1) according to the requirement of Ultra-low carbon content range, in the 0.0005-0.005% content range, design certain concentration gradients, base is got at smelting, ingot casting or factory scene, removes the peel, forges rod appearance according to general standard material work flow;
2) turning is processed into granular or the sheet sample, controls every gram granule number at 200-600, promptly roughly is equivalent to the 0.6-0.8mm cuboid sample.The purpose of control granularity: controlling on the one hand granularity, to be of value to down in the operation coating even, promptly is of value to the homogeneity of standard substance; Meticulous on the other hand or cross the adverse effect of bulk specimen to high-frequency induction.That process prevents is overheated, sample does not grind, and purpose is homogeneity and the surface oxidation influence firmness of operation coating down that prevents the inhomogeneous oxidation affects standard substance of specimen surface.
3) with the sample after the car system according to the general industry technological process zinc-plated or nickel.Zinc-plated or nickel is the technical measures that economic, general iron is prevented atmospheric corrosion.After zinc-plated, the ability of the anti-atmospheric corrosion of sample improves in more than 20 times, and the widespread use in the oxygen standard substance in steel of nickel plating sample weather-resistance, metallurgical analysis circle has the use experience of decades.
4) simulation test shows: after sample zinc-plated or nickel was soaked in water, anti-corrosion capability received appreciable impact in atmosphere.Adopt in the steel of present patent application preparation the Ultra-low carbon standard substance must adopt glass, the plastic bottle encapsulation of band inner cap or join sealed paper in addition and close external packing, to guarantee the general 10 year shelf-life that requires of standard substance.
5) use the standard substance of present technique development, the Ultra-low carbon infrared analysis of the production sample of behind block specimen preparation, directly measuring to be measured, can proofread and correct by conventional method, conventional method mensuration, measured value is consistent with preheating method.
The present invention is for resolving the formation of specimen surface carbon; With sample (comprising production to be measured appearance and standard substance) in 420 ℃ of thermal pretreatment after 10 minutes; Move to and be cooled to room temperature in the exsiccator; And in one, two day, measure its carbon content (hereinafter to be referred as the preheating cooling method), and make comparisons with the preheating method (directly measuring after the sample preheating) and the measured value of conventional method (sample is thermal pretreatment not), test findings of producing appearance and standard substance to be measured is seen table 1, table 2 respectively:
Table 1 carbon measured value (%) of producing under the different pre-treatment modes of appearance to be measured
| Production sample to be measured | Preheating method | Conventional method | The present invention |
| Production appearance 1 to be measured | 0.0013 | 0.0015 | 0.0015 |
| Production appearance 2 to be measured | 0.0014 | 0.0016 | 0.0015 |
| Production appearance 3 to be measured | 0.0020 | 0.0022 | 0.0022 |
| Production appearance 4 to be measured | 0.0056 | 0.0058 | 0.0057 |
| Production appearance 5 to be measured | 0.0069 | 0.0071 | 0.0070 |
| Production appearance 6 to be measured | 0.0071 | 0.0075 | 0.0073 |
| Production appearance 7 to be measured | 0.0096 | 0.0100 | 0.0098 |
Carbon measured value (%) under the different pre-treatment modes of table 2 standard substance
| The standard substance trade mark | Preheating method | Conventional method | The preheating cooling method |
| YSBS20143 | 0.0084 | 0.0090 | 0.0086 |
| YSBS20144 | 0.0019 | 0.0025 | 0.0022 |
| YSBS20125 | 0.0069 | 0.0074 | 0.0072 |
| JSS1205-1 | 0.0008 | 0.0010 | 0.0009 |
| GSB03-1566 | 0.0014 | 0.0019 | 0.0017 |
| GSB1671 | 0.0014 | 0.0017 | 0.0015 |
| GBW1402e | 0.0001 | 0.0010 | 0.0003 |
Claims (2)
1. the preparation method of a ultra-low-carbon steel standard substance is characterized in that, it comprises the following steps:
1) according to the requirement of Ultra-low carbon content range, in the 0.0005-0.005% content range, design certain concentration gradients, base is got at smelting, ingot casting or factory scene, removes the peel, forges rod appearance;
2) turning is processed into granular or the sheet sample, controls every gram granule number at 200-600, and that process need prevent is overheated, must not grind sample;
3) the zinc-plated or nickel with the sample after the car system;
4) glass of employing band inner cap, plastic bottle encapsulate or join sealed paper box package sample in addition, to guarantee the general 10 year shelf-life that requires of standard substance.
2. one kind is adopted the described ultra-low-carbon steel standard substance of claim 1 to measure corresponding Ultra-low carbon content method, it is characterized in that, adopts conventional method to measure its carbon content jointly production appearance to be measured and standard substance.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04160349A (en) * | 1990-10-25 | 1992-06-03 | Nkk Corp | Apparatus for simultaneous analysis of c and s |
| JPH10183322A (en) * | 1996-12-24 | 1998-07-14 | Nisshin Steel Co Ltd | Galcannealed steel sheet for coating |
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2010
- 2010-12-06 CN CN2010105739079A patent/CN102486442A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04160349A (en) * | 1990-10-25 | 1992-06-03 | Nkk Corp | Apparatus for simultaneous analysis of c and s |
| JPH10183322A (en) * | 1996-12-24 | 1998-07-14 | Nisshin Steel Co Ltd | Galcannealed steel sheet for coating |
Non-Patent Citations (2)
| Title |
|---|
| 李小杰，周大庆，胡涛: "超低碳钢的取样和制样方法", 《武钢技术》, vol. 38, no. 2, 31 March 2000 (2000-03-31) * |
| 陈桓庆: "微量碳定量用钢铁标准物质的制备及其认证值的确定", 《冶金标准化与质量》, vol. 1, no. 1, 31 December 1996 (1996-12-31) * |
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Application publication date: 20120606 |