CN113188862A - Method for measuring content of dissolved elements in molten steel - Google Patents
Method for measuring content of dissolved elements in molten steel Download PDFInfo
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- CN113188862A CN113188862A CN202110344528.0A CN202110344528A CN113188862A CN 113188862 A CN113188862 A CN 113188862A CN 202110344528 A CN202110344528 A CN 202110344528A CN 113188862 A CN113188862 A CN 113188862A
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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Abstract
A method for measuring the content of dissolved elements in molten steel relates to the field of chemical detection of ferrous metallurgy and comprises the following steps: s1: cooling a liquid molten steel sample to be measured to prepare a solid steel sample; s2: placing the solid steel sample into electrolyte for electrochemical corrosion, and measuring the mass change delta m of the solid steel sample before and after the electrochemical corrosionsteel(ii) a S3: removing nonmetallic inclusions in the electrolyte after electrochemical corrosion to obtain an element solution to be detected; s4: determining the mass m of the dissolved element i in the element solution to be detectedi(ii) a S5: obtaining the mass fraction of the dissolved element i in the liquid molten steel to be detected
The method effectively separates elements in non-metallic inclusion in steel from dissolved elements in steel by electrochemical corrosion, filtration and other methods, and then dissolves elements in electrochemical corrosion solutionThe chemical analysis of the element content is carried out by ICP, the measuring method has accurate precision, and the effective measurement of the content of dissolved elements in the steel can be realized.
Description
Technical Field
The invention relates to the field of chemical detection of ferrous metallurgy, in particular to a method for measuring the content of dissolved elements in molten steel.
Background
The alloy content is one of the important indexes of steel materials, and directly influences the quality and the product performance of steel. The addition of the effective alloy elements into the steel can effectively reduce the content of the oxygen element impurity in the steel, modify the nonmetallic inclusion in the steel and improve the product performance of the steel material. The elements in the steel material include two parts of dissolved elements in molten steel and elements in non-metallic inclusions in steel, and the sum of the two parts is called the total element content. The content of the dissolved elements can be applied to thermodynamic prediction of reaction among slag, steel and inclusions, and is an important parameter for realizing accurate calculation and prediction of components in the steelmaking process. However, only the total element content in steel can be measured and analyzed in China at present, and no effective method for measuring the content of dissolved elements in molten steel exists. On the one hand, the change of dissolved elements in the steel during the solidification and cooling processes of the steel is ignored, and a proper cooling mode is not adopted for the sample; on the other hand, because both steel and non-metallic inclusions are easily dissolved in acid, no suitable method for extracting dissolved elements in steel and elements in non-metallic inclusions is found. The prior patent proposes a method for measuring solid solution elements in steel by measuring the solid solution elements in a slowly cooled steel sample, however, the method for measuring the solid solution elements does not consider that the dissolved elements in molten steel and non-metallic inclusions in the steel are subjected to chemical reaction in the process of slow solidification and cooling of the steel, so that the content of elements finally remained in the steel is changed, and is different from the content of the dissolved elements in initial liquid molten steel. Therefore, it is necessary to provide a method for measuring the content of dissolved elements in molten steel.
Disclosure of Invention
The invention provides a method for measuring the content of dissolved elements in molten steel, which effectively separates elements in nonmetallic inclusions in steel from dissolved elements in the steel by using methods such as electrochemical corrosion, filtration and the like, and then carries out chemical analysis on the content of the dissolved elements in an electrochemical corrosion solution through ICP (inductively coupled plasma), and the measuring method has accurate precision and can realize effective measurement on the content of the dissolved elements in the steel.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for measuring the content of dissolved elements in molten steel comprises the following steps:
s1: cooling a liquid molten steel sample to be measured to prepare a solid steel sample;
s2: placing the solid steel sample into electrolyte for electrochemical corrosion, and measuring the mass change delta m of the solid steel sample before and after the electrochemical corrosionsteel；
S3: removing nonmetallic inclusions in the electrolyte after electrochemical corrosion to obtain an element solution to be detected;
s4: determining the mass m of the dissolved element i in the element solution to be detectedi；
S5: obtaining the mass fraction of the dissolved element i in the liquid molten steel to be detected
Further, the electrolyte is methanol solution of triethanolamine, glycerol, tetramethylammonium chloride and acetylacetone.
Further, in the electrolyte, the mass percentage of triethanolamine is 1-15%, the mass percentage of glycerol is 1-15%, the mass percentage of tetramethylammonium chloride is 0.01-5%, and the mass percentage of acetylacetone is 0.01-5%.
Further, the cooling rate in S1 is more than 10 ℃/min.
Further, the S3 specifically includes: filtering and removing nonmetallic inclusions containing dissolved elements to be detected in the electrolyte after electrochemical corrosion by using filter paper to obtain an element solution to be detected;
wherein the porosity of the filter paper is 0.5-1 μm.
Further, the S4 specifically includes: quantitatively measuring the mass m of the dissolved element i in the element solution to be measured by an inductively coupled plasma emission spectrometeri；
The content range of the measuring elements of the inductively coupled plasma emission spectrometer is 0.0005-5%, and the measuring precision is 0.00001%.
Further, the temperature of the liquid molten steel sample to be measured in S1 is more than 1500 ℃.
Further, the dissolved elements comprise one or more of Ca, Mg, Ti, Si and Mn.
Further, the solid steel sample is a cylinder, the diameter of the solid steel sample is 11-15 mm, and the height of the solid steel sample is 110-150 mm.
Further, in the electrochemical corrosion process of S2, the corrosion voltage is 20-200 mV, the corrosion current is 10-100 mA, the corrosion temperature is-10 to-5 ℃, the corrosion atmosphere is inert gas, and the corrosion time is 60-90 minutes.
Compared with the prior art, the method for measuring the content of the dissolved elements in the molten steel has the following advantages: the invention provides a new method for measuring the content of dissolved elements in molten steel, which is characterized in that a high-temperature liquid molten steel sample is sampled and rapidly cooled to room temperature, so that the chemical reaction between the dissolved elements in the molten steel and non-metallic inclusions in steel is avoided, the content of the dissolved elements in the initial liquid molten steel sample is ensured not to change in the cooling process, the non-metallic inclusions in the steel and the steel are separated by an electrolysis method in order to avoid the influence of the dissolution of the non-metallic inclusions in an acid solution on the measurement result, and elements in the non-metallic inclusions in the steel and the dissolved elements in the steel are separated by electrochemical corrosion by taking a methanol solution of triethanolamine, glycerol, tetramethylammonium chloride and acetylacetone as an electrochemical corrosion solution. And filtering the mixture by filter paper with the porosity of 0.5-1 mu m to prevent the loss of inclusions containing the tested elements. The content of the dissolved elements in the steel is chemically analyzed by an inductively coupled plasma emission spectrometer, the measuring method is accurate in precision, and the content of the dissolved elements in the steel can be effectively measured.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
In the drawings:
FIG. 1 is a schematic flow chart of the measurement method of the present invention.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the invention, as detailed in the appended claims.
The terms first, second and the like in the description and in the claims of the present invention are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are, for example, capable of operation in sequences other than those illustrated or otherwise described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
A plurality, including two or more.
And/or, it should be understood that, as used herein, the term "and/or" is merely one type of association that describes an associated object, meaning that three types of relationships may exist. For example, a and/or B, may represent: a exists alone, A and B exist simultaneously, and B exists alone.
A method for measuring the content of dissolved elements in molten steel effectively separates elements in nonmetallic inclusions in the steel from the dissolved elements in the steel, and comprises the following specific steps:
(1) sampling a high-temperature liquid molten steel sample, and rapidly cooling to room temperature;
(2) the steel samples were formed into round bars and weighed.
(3) Using methanol solution of triethanolamine, glycerol, tetramethylammonium chloride and acetylacetone as electrochemical corrosion solution, carrying out corrosion separation on dissolved elements and elements in inclusions in steel materials by an electrochemical corrosion method, quantitatively weighing the mass difference of the dried steel sample before and after electrochemical corrosion, and determining the mass delta m of electrolytically corroded steelsteel；
(4) Removing nonmetallic inclusions containing test elements by a filtering method to obtain an electrochemical corrosion solution;
(5) quantitative determination of certain dissolved element content m in electrochemical corrosion solution by inductively coupled plasma emission spectrometeri；
(6) Obtaining w by formulai＝mi/△msteelAnd obtaining the mass fraction of a certain dissolved element i in the steel sample.
Preferably, the cooling rate of the molten steel sample in the step (1) is more than 10 ℃/min, so that dissolved elements in the molten steel are prevented from participating in chemical reaction with nonmetallic inclusions in the steel in the process of solidifying and cooling the molten steel.
Preferably, the steel sample round bar in the step (2) has a diameter of 11-15 mm and a height of 110-150 mm, so that subsequent electrolysis parameters are controlled stably, the overlarge round bar is not beneficial to uniform and rapid electrolysis of the solution, and the undersized round bar is not beneficial to element measurement quantification.
Preferably, in the methanol solution of triethanolamine, glycerol, tetramethylammonium chloride and acetylacetone in the step (3), the mass percentage of the triethanolamine is 1-15%, the mass percentage of the glycerol is 1-15%, the mass percentage of the tetramethylammonium chloride is 0.01-5%, and the mass percentage of the acetylacetone is 0.01-5%.
Preferably, in the electrochemical corrosion method in the step (3), the corrosion voltage is 20-200 mV, the corrosion current is 10to 100mA, the corrosion temperature is-10 to-5 ℃, the corrosion atmosphere is argon, and the corrosion time is 60-90 minutes.
Preferably, in the filtering method in the step (4), the porosity of the filter paper is 0.5-1 μm, so that the loss of the inclusion containing the test element is prevented.
Preferably, in the inductively coupled plasma emission spectrometer in the step (5), the content of the measuring element ranges from 0.0005 to 5%, and the requirement on the measuring precision reaches 0.00001%.
Example (b): (chemical composition of steel sample (mass%) C0.998%, Si 0.201%, Mn 0.359% Cr 1.44%, S0.003%, Al 0.0149%, T.Mg 0.0003%, T.Ca 0.0011%, T.O 0.0008%, and the balance Fe, wherein the content of dissolved calcium is 0.00015%, and T.Mg, T.Ca and T.O respectively represent the total magnesium, calcium and oxygen contents in steel)
As shown in figure 1, 1600 ℃ molten steel is sampled and then rapidly cooled to room temperature at the speed of 50 ℃/min, and a steel sample is processed into a round bar with the diameter of 11mm and the height of 110mm and weighed; 250ml of methanol solution of triethanolamine, glycerol, tetramethylammonium chloride and acetylacetone is taken as electrochemical corrosion solution, wherein the mass percentage of the triethanolamine is 3%, the mass percentage of the glycerol is 3%, the mass percentage of the tetramethylammonium chloride is 1%, and the mass percentage of the acetylacetone is 1%; and carrying out corrosion separation on calcium dissolved in the weighed steel material and calcium in the inclusions by an electrochemical corrosion method, wherein the corrosion voltage is 100mV, the corrosion current is 50mA, the corrosion temperature is-10 to-5 ℃, the corrosion atmosphere is argon, and the corrosion time is 60 minutes. Cleaning the electrolyzed sample, drying and weighing the sample, and determining the quality delta m of the electrolytically corroded steelsteel5.1 g; removing calcium oxide-containing nonmetallic inclusions by a filter paper filtering method with the porosity of 1 mu m to obtain an electrochemical corrosion solution; quantitatively measuring the content m of dissolved calcium in the electrochemical corrosion solution by an inductively coupled plasma emission spectrometerCaAt 32.15. mu.g, w is obtained by using the formulaCa＝mCa/△msteelThe mass fraction of the dissolved calcium Ca in the obtained steel sample is 0.00063%. Cleaning the electrolyzed sample, drying and weighing the sample, and determining the quality delta m of the electrolytically corroded steelsteel5.2 g; removing calcium oxide-containing nonmetallic inclusions by a filter paper filtering method with the porosity of 1 mu m to obtain an electrochemical corrosion solution; quantitatively measuring the content m of dissolved calcium in the electrochemical corrosion solution by an inductively coupled plasma emission spectrometerCaAt 8.42. mu.g, w is obtained by using the formulaCa＝mCa/△msteelThe mass fraction of the dissolved calcium Ca in the obtained steel sample is 0.00016%.
Comparative example: (chemical composition of steel sample (mass%) C0.998%, Si 0.201%, Mn 0.359% Cr 1.44%, S0.003%, Al 0.0149%, T.Mg 0.0003%, T.Ca 0.0011%, T.O 0.0008%, and the balance Fe, in which the content of dissolved calcium is 0.00015%)
Sampling molten steel at 1600 ℃, slowly cooling to room temperature at a speed of less than 5 ℃/min, processing a steel sample with dissolved calcium content of 0.00016% into a round bar with the diameter of 11mm and the height of 110mm, and weighing; 250ml of methanol solution of triethanolamine, glycerol, tetramethylammonium chloride and acetylacetone is taken as electrochemical corrosion solution, wherein the mass percentage of the triethanolamine is 3%, the mass percentage of the glycerol is 3%, the mass percentage of the tetramethylammonium chloride is 1%, and the mass percentage of the acetylacetone is 1%; and carrying out corrosion separation on calcium dissolved in the weighed steel material and calcium in the inclusions by an electrochemical corrosion method, wherein the corrosion voltage is 100mV, the corrosion current is 50mA, the corrosion temperature is-10 to-5 ℃, the corrosion atmosphere is argon, and the corrosion time is 60 minutes. Cleaning the electrolyzed sample, drying and weighing the sample, and determining the quality delta m of the electrolytically corroded steelsteel5.1 g; removing calcium oxide-containing nonmetallic inclusions by a filter paper filtering method with the porosity of 1 mu m to obtain an electrochemical corrosion solution; quantitatively measuring the content m of dissolved calcium in the electrochemical corrosion solution by an inductively coupled plasma emission spectrometerCaAt 3.22. mu.g, w is obtained by using the formulaCa＝mCa/△msteelThe mass fraction of the dissolved calcium Ca in the obtained steel sample is 0.000063%. The measured value of the dissolved calcium content is significantly lower than its standard value of 0.00015%. The main reason is that the molten steel is slowly cooled to room temperature from 1600 ℃ at a speed of less than 5 ℃/min, and the slow cooling leads to more time for dissolving element calcium in the molten steel to react with nonmetallic inclusions in the steel to generate inclusions, so that the content of the dissolved calcium in the steel with a measurement result is obviously reduced, and the content of the dissolved calcium in the molten steel cannot be truly reflected.
The above-mentioned serial numbers of the embodiments of the present invention are merely for description and do not represent the merits of the embodiments.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for measuring the content of dissolved elements in molten steel is characterized by comprising the following steps:
s1: cooling a liquid molten steel sample to be measured to prepare a solid steel sample;
s2: placing the solid steel sample into electrolyte for electrochemical corrosion, and measuring the mass change delta m of the solid steel sample before and after the electrochemical corrosionsteel；
S3: removing nonmetallic inclusions in the electrolyte after electrochemical corrosion to obtain an element solution to be detected;
s4: determining the mass m of the dissolved element i in the element solution to be detectedi；
S5: obtaining the mass fraction of the dissolved element i in the liquid molten steel to be detected
2. The method for measuring the content of dissolved elements in molten steel according to claim 1, wherein the electrolyte is a methanol solution of triethanolamine, glycerol, tetramethylammonium chloride and acetylacetone.
3. The method for measuring the content of the dissolved elements in the molten steel according to claim 2, wherein in the electrolyte, the mass percent of triethanolamine is 1-15%, the mass percent of glycerol is 1-15%, the mass percent of tetramethylammonium chloride is 0.01-5%, and the mass percent of acetylacetone is 0.01-5%.
4. The method as claimed in claim 1, wherein the cooling rate in S1 is greater than 10 ℃/min.
5. The method for measuring the content of the dissolved element in the molten steel according to claim 1, wherein the step S3 specifically comprises: filtering and removing nonmetallic inclusions containing dissolved elements to be detected in the electrolyte after electrochemical corrosion by using filter paper to obtain an element solution to be detected;
wherein the porosity of the filter paper is 0.5-1 μm.
6. The method for measuring the content of the dissolved element in the molten steel according to claim 1, wherein the step S4 specifically comprises: quantitatively measuring the mass m of the dissolved element i in the element solution to be measured by an inductively coupled plasma emission spectrometeri；
The content range of the measuring elements of the inductively coupled plasma emission spectrometer is 0.0005-5%, and the measuring precision is 0.00001%.
7. The method as claimed in claim 1, wherein the temperature of the liquid steel sample to be measured in S1 is more than 1500 ℃.
8. The method of claim 1, wherein the dissolved elements comprise one or more of Ca, Mg, Ti, Si, and Mn.
9. The method for measuring the content of the dissolved elements in the molten steel according to claim 1, wherein the solid steel sample is a cylinder, and the diameter of the solid steel sample is 11-15 mm, and the height of the solid steel sample is 110-150 mm.
10. The method for measuring the content of the dissolved elements in the molten steel according to claim 1, wherein in the electrochemical corrosion process of S2, the corrosion voltage is 20-200 mV, the corrosion current is 10-100 mA, the corrosion temperature is-10 to-5 ℃, the corrosion atmosphere is inert gas, and the corrosion time is 60-90 minutes.
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