Particle steel component detection method

Abstract

The invention relates to the technical field of material detection in the iron and steel industry, in particular to a particle steel component detection method which comprises the following steps: (1) heating and melting a particle steel sample to be detected to obtain metal 1 and slag 1, and detecting the percentage content of an element M in the metal 1; (2) taking powder of an element M as a doped alloy, and detecting the percentage content of the element M in the doped alloy; (3) taking another part of particle steel sample to be detected in the same batch as that in the step (1), mixing the particle steel sample to be detected with the doped alloy, and heating and melting to obtain metal 2 and slag 2; (4) detecting the percentage composition of an element M and a to-be-detected element in the metal 2 and the percentage composition of the to-be-detected element in the slag 2; and (5) calculating the mass of the metal 2 and the mass of the slag 2 in the to-be-detected sample of the particle steel in the step (3) according to the following formula, and finally calculating the percentage content of the to-be-detected element in the particle steel. The method solves the problems that metal in particle steel cannot be ground into powder, and components cannot be detected by using a conventional detection method.

Description

Technical Field

[0001] The present invention relates to the technical field of material detection in the iron and steel industry, and particularly relates to a method for detecting the composition of granular steel. Background Art

[0002] Granular steel is a by-product of the iron and steel industry and the manufacturing industry. Its main sources include the products after steel slag separation, the oxidized slag from flame cutting of steel, welding iron oxide, and iron filings after cold processing of steel. Granular steel contains metallic iron and iron oxides, with an iron content between 60% and 85%. It is generally recycled as low-quality scrap steel in processes such as converters, electric furnaces, and induction furnaces.

[0003] When traditional iron ore-containing materials are subjected to composition detection, they are generally crushed to less than 100 mesh or made into polished slices, and then directly analyzed using chemical analysis methods or spectroscopic methods. However, since granular steel is a mixture of metals and non-metals, and the metals have ductile properties, the existing processing means cannot process the granular steel sample to less than 100 mesh, so it cannot meet the requirements of the sample specifications for detection. Currently, the melting separation method is mainly used to determine the quality of granular steel, that is, the melting and water discharge rate. This method is difficult to completely separate the metal from the molten slag, and there are problems such as carburization. The detection accuracy is low, and there is a lack of composition detection, which cannot well meet the detection requirements for the effective components of economic scrap steel.

[0004] Chinese Patent Application CN 113720725 A discloses a method for detecting granular steel. First, a pure steel sample is melted to obtain a first molten steel, and the composition of the first molten steel is analyzed; then the granular steel sample is mixed and melted with the first molten steel to obtain a second molten steel and molten slag, and the compositions of the second molten steel and molten slag are analyzed; then, according to the weight of the pure steel sample, the weight of the granular steel sample, the weight of the second molten steel, and the weight of the molten slag, the percentage content of the composition of the granular steel sample is calculated. The disadvantage of this method is that it is necessary to separately measure the weight T3 of the second molten steel and the weight T4 of the molten slag, and the accuracy of the result largely depends on the separation degree of the second molten steel and the molten slag, but this technical solution does not record how it processes the second molten steel and the molten slag. In actual measurement, completely separating the molten slag and the molten steel has always been a difficult point in operation. Therefore, using this technical solution to measure the composition of granular steel is prone to large errors. Summary of the Invention

[0005] Aiming at the technical problem that the melting separation method cannot well meet the detection requirements for the effective components of economic scrap steel, the present invention provides a method for detecting the composition of granular steel, which uses the measurement of the change in the composition of doped elements to calculate the composition of granular steel, effectively avoiding the difficult problem of separating molten steel and molten slag.

[0006] The technical solution of the present invention is as follows: A method for detecting the composition of granular steel, comprising the following steps: (1)Take a particle steel sample to be inspected with a mass of G 1 and heat it to melting to obtain separated metal 1 and slag 1. After cooling, detect the percentage content A of element M in metal 1 through an X-ray fluorescence analyzer 1 ; Element M is an element that dissolves in Fe but does not react with air, the container, and the substances contained in the particle steel; (2)Take a powder of element M with a mass of G 2 as a doped alloy, and detect the percentage content A of element M in the doped alloy through an X-ray fluorescence analyzer 2 ; (3)Take another particle steel sample to be inspected with the same batch as in step (1) and with a mass of G 1 , mix it with the doped alloy in step (2) and heat it to melting to obtain completely separated metal 2 and slag 2; (4)After cooling, detect the percentage content A of element M in metal 2 3 , the percentage content B of the element to be detected in metal 2 1 and the percentage content B of the element to be detected in slag 2 2 ; (5)Calculate the mass G 1 of the metal in the particle steel sample to be inspected with a mass of G 3 , the mass G 4 of slag 2 obtained in step (3), and finally obtain the percentage content C of the element to be detected in the particle steel: , , .

[0007] Furthermore, element M is selected from Cu, Ni, Co, Au, Pt or Wu.

[0008] Furthermore, in step (1), heat and hold for 30 minutes at 1550 °C, and then cool naturally. The heating and holding process and the natural cooling process are both carried out in a protective atmosphere.

[0009] Furthermore, in step (3), heat and hold for 30 minutes at 1550 °C, and then cool naturally. The heating and holding process and the natural cooling process are both carried out in a protective atmosphere.

[0010] Furthermore, the protective atmosphere is a nitrogen atmosphere.

[0011] Furthermore, in step (3), rotate and shake the particle steel sample to be inspected and the doped alloy for 5 minutes.

[0012] Furthermore, the element to be detected is selected from Fe, C, Si, Mn, P, S, Mg, Al or Ca.

[0013] Furthermore, generally, the detection of granular steel focuses on the content of Fe element. Therefore, when there is no clear requirement for the content of C element in granular steel, a graphite crucible can be used as the container and heated in an intermediate frequency furnace. Compared with a resistance furnace, the intermediate frequency furnace has a high heating efficiency, which can effectively shorten the detection time and improve the detection efficiency.

[0014] The beneficial effects of the present invention are as follows: (1) Introduce the element M for determining the composition to calibrate the composition of the test sample, which has no influence on the test sample during the detection process; (2) Solve the problems that it is impossible to prepare samples and it is difficult to completely separate metal and slag during the detection of granular steel; (3) Can completely measure the contents of Fe, C, Si, Mn, P, S, Mg, Al, and Ca in granular steel, and simultaneously determine the accurate weight of the metal components in granular steel; (4) This method has high precision and is easy to operate; (5) This method can also be applied to the detection of the composition of similar metal and non-metal mixtures. Specific embodiments

[0015] In order to enable those skilled in the art to better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0016] Example 1 A method for detecting the composition of granular steel includes the following steps: (1) Take a granular steel test sample with a mass G 1 = 150 g and heat it to melt. Place it in a magnesia crucible and heat it to 1550 °C in a high-temperature resistance furnace under a nitrogen atmosphere. After keeping it at a constant temperature for 30 minutes, turn off the heating power supply and naturally cool it to room temperature under a nitrogen atmosphere to obtain completely separated metal 1 and slag 1. Detect the percentage content A of Cu element in metal 1 through an X-ray fluorescence analyzer 1 ; (2) Take 10 g of analytical pure Cu powder as a doped alloy with a mass G 2 and detect the percentage content A of Cu element in the doped alloy through an X-ray fluorescence analyzer 2 = 99.9%; (3) Take another batch with the same quality as in step (1) and with a mass of G 1, that is, a 150 g particle steel sample to be tested, is placed in a magnesia crucible together with the doped alloy in step (2), shaken and rotated for 5 minutes, then heated to 1550 °C in a high-temperature resistance furnace under a nitrogen atmosphere, held at a constant temperature for 30 minutes, the heating power is turned off, and it is naturally cooled to room temperature under a nitrogen atmosphere to obtain completely separated metal 2 and slag 2; (4) Detect the percentage content A of Cu element in metal 2 by an X-ray fluorescence analyzer 3 , the percentage content B of the element to be detected in metal 2 1 and the percentage content B of the element to be detected in slag 2 2 ; (5) Calculate according to the following formula the mass G 1 of the metal in the particle steel sample to be tested with a mass of G 3 , the mass G 4 of slag 2, and finally obtain the percentage content C of the element to be detected in the particle steel. The element to be detected is selected from Fe, C, Si, Mn, P, S, Mg, Al or Ca: , , .

[0017] At the same time, the mass G 5 of the metal components of the particle steel can also be calculated, that is, the melting and clearing water yield, and the calculation formula is: .

[0018] Example 2 Verify the accuracy of the particle steel composition detection method of the present invention. The verification method is as follows: (1) Take an analytical pure iron powder with a mass G 1 = 150 g, and detect the iron powder composition by an X-ray fluorescence analyzer as shown in Table 1, where the percentage content A 1 of Fe element = 99.242%; (2) Take 7 g of analytical pure Cu powder as the doped alloy, and detect the doped alloy composition by an X-ray fluorescence analyzer as shown in Table 1, where the percentage content A 2 of Cu element = 99.833%; 2 = 99.833%; (3) Place the iron powder and copper powder in a graphite crucible, shake and rotate for 5 minutes, then heat to 1550 °C in a high-temperature resistance furnace under a nitrogen atmosphere, hold at a constant temperature for 30 minutes, turn off the heating power, and naturally cool to room temperature under a nitrogen atmosphere to obtain an iron-copper alloy ingot; (4) Detect the percentage content A 3is 4.466%, and the percentage content B of Fe element in the iron-copper alloy ingot Fe is 95.201%; (5) Calculate the mass G of the pure iron powder metal according to the following formula 3 (Calculated mass). Since the materials used in this verification test are all pure metals, the mass G of the slag is recorded 4 = 0, and finally the percentage content Fe (calculated concentration) of the element to be measured in the iron powder is obtained.

[0019] , .

[0020] (6) The actual values and the detected values are shown in Table 1.

[0021] Table 1 Actual concentrations and calculated concentrations of iron powder, copper powder and iron-copper alloy ingots

[0022] Although the present invention has been described in detail by combining preferred embodiments, the present invention is not limited thereto. Without departing from the spirit and essence of the present invention, those of ordinary skill in the art can make various equivalent modifications or substitutions to the embodiments of the present invention, and these modifications or substitutions should all be within the scope of the present invention / Any person skilled in the art within the technical scope disclosed by the present invention can easily think of changes or substitutions, which should all be covered by the protection scope of the present invention.

Claims

1. A method for detecting the composition of particle steel, characterized in that: The steps include: (1) Take a particle steel sample with a mass of G1 and heat it to melt it to obtain completely separated metal 1 and slag 1. After cooling, use an X-ray fluorescence analyzer to detect the percentage content A1 of element M in metal 1; Element M is an element that dissolves in Fe but does not react with the air, the container, and the substances contained in the particle steel; (2) Take a powder of element M with a mass of G2 as a doped alloy, and use an X-ray fluorescence analyzer to detect the percentage content A2 of element M in the doped alloy; (3) taking another sample of the particle steel to be tested of mass G1 from the same batch as step (1), mixing it with the doped alloy from step (2), and then heating and melting it to obtain separated metal 2 and slag 2; (4) After cooling, the percentage content A3 of the element M in the metal 2, the percentage content B1 of the element to be tested in the metal 2, and the percentage content B2 of the element to be tested in the slag 2 are detected by an X-ray fluorescence analyzer; (5) Calculate the mass G3 of the metal in the particle steel sample to be tested and the mass G4 of the slag 2 with a mass of G1 according to the following formula, and finally obtain the percentage content C of the element to be tested in the particle steel: ， ， 。 2. The particle steel composition detection method according to claim 1, characterized in that: The element M is selected from Cu, Ni, Co, Au, Pt or Wu.

3. The particle steel composition detection method according to claim 1, characterized in that: In step (1), the mixture is heated and kept at 1550° C. for 30 minutes and then cooled naturally. The heating, keeping and natural cooling processes are all carried out in a protective atmosphere.

4. The particle steel composition detection method according to claim 1, characterized in that: In step (3), the mixture is heated and kept at 1550° C. for 30 minutes and then cooled naturally. The heating, keeping and natural cooling processes are both carried out in a protective atmosphere.

5. The particle steel component detection method according to claim 3 or 4, characterized in that: The protective atmosphere was nitrogen.

6. The particle steel composition detection method according to claim 1, characterized in that: In step (3), the particle steel sample to be tested and the doped alloy are rotated and shaken for 5 minutes.

7. The particle steel composition detection method according to claim 1, characterized in that: The element to be measured is selected from Fe, C, Si, Mn, P, S, Mg, Al or Ca.

8. The particle steel composition detection method according to claim 1, characterized in that: A graphite crucible is used as a container and heated in a medium frequency furnace.

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