CN117554355A - Method for accurately measuring content of acid-soluble aluminum in steel - Google Patents
Method for accurately measuring content of acid-soluble aluminum in steel Download PDFInfo
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- CN117554355A CN117554355A CN202311564277.2A CN202311564277A CN117554355A CN 117554355 A CN117554355 A CN 117554355A CN 202311564277 A CN202311564277 A CN 202311564277A CN 117554355 A CN117554355 A CN 117554355A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 64
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 41
- 239000010959 steel Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000004458 analytical method Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 230000005284 excitation Effects 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004993 emission spectroscopy Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 description 14
- 229910000976 Electrical steel Inorganic materials 0.000 description 11
- 238000001514 detection method Methods 0.000 description 10
- 238000005259 measurement Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 229910000851 Alloy steel Inorganic materials 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000001636 atomic emission spectroscopy Methods 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 229910000975 Carbon steel Inorganic materials 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000010962 carbon steel Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 238000005261 decarburization Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
-
- 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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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention belongs to the technical field of steel material chemical analysis, and discloses a method for accurately measuring the content of acid-soluble aluminum in steel. Firstly, taking a block-shaped steel sample, placing the block-shaped steel sample on an excitation table of a spark discharge atomic emission spectrometer, and measuring an acid-soluble aluminum content reference value; secondly, taking a chip-shaped steel sample, adding a mixed solution of nitric acid and hydrochloric acid, adding perchloric acid after the chip-shaped steel sample is dissolved, heating for dissolving, determining the heating temperature and time according to an acid-soluble aluminum content reference value detected by a spark discharge atomic emission spectrometer, and cooling to a constant volume after heating is finished to obtain a solution to be measured; and finally, introducing the solution to be measured into an inductively coupled plasma atomic emission spectrometer, and determining the content of the obtained acid-soluble aluminum as an accurate determination result. According to the invention, through accurately grasping the temperature and time of the dissolved sample in the measuring process of the inductively coupled plasma emission spectrometry, the accurate measuring result of the acid-soluble aluminum content is obtained, and the accuracy is controlled within +/-3 ppm.
Description
Technical Field
The invention belongs to the technical field of steel material chemical analysis, and particularly relates to a method for accurately measuring the content of acid-soluble aluminum in steel.
Background
Aluminum has important influence on the performance of many steel grades, aluminum exists in steel in two states of acid-soluble aluminum and acid-insoluble aluminum, and the state and the content of aluminum need to be strictly controlled in the production process of the steel, so that accurate determination of aluminum in the steel becomes an indispensable task.
Particularly for oriented silicon steel, accurate determination of the acid-soluble aluminum content is particularly important. Acid-soluble aluminum in the oriented silicon steel is a main element for forming an AlN inhibitor, the amount of generated AlN is small when the content of the acid-soluble aluminum is low, and normal growth of primary recrystallization grains cannot be prevented, so that good secondary recrystallization cannot be performed; if the acid-soluble aluminum content is too high, alN is not sufficiently solid-dissolved even if the solid-solution treatment is performed before hot rolling due to the relationship of the solid-solution amount of AlN, and even if the annealing is performed in a nitrogen atmosphere, good secondary recrystallization cannot be performed. Therefore, the control range of the acid-soluble aluminum of the oriented silicon steel is gradually narrowed, and as the acid-soluble aluminum content is the main basis for making a post-process, the magnetic performance of the oriented silicon steel final product is determined, and the accuracy requirement on the acid-soluble aluminum detection is also gradually improved.
The determination of the acid-soluble aluminum content in the conventional steel grade mainly adopts the national standard GB/T20125-2006 "determination of the multi-element content of low alloy steel" inductively coupled plasma emission spectrometry ", and utilizes the characteristic that acid-soluble aluminum can be decomposed by inorganic acid, firstly, the acid is used for dissolving the acid, and then the inductively coupled plasma atomic emission spectrometry is used for determination. However, practical results prove that the sample dissolution temperature and the sample dissolution time have great influence on the detection result, the result is lower due to the fact that the sample dissolution temperature is too low and the sample dissolution time is too short, and the result is higher due to the fact that a small amount of acid insoluble aluminum is dissolved when the sample dissolution temperature is too high and the sample dissolution time is too long, so that the accuracy of the detection result is difficult to guarantee.
Besides the inductively coupled plasma emission spectrometry, the method is also a common method, namely, a national standard GB/T4336-2016 (carbon steel and middle and low alloy steel multi-element content determination spark discharge atomic emission spectrometry (conventional method)) is originally used for determining the content of all aluminum in steel, but with the improvement of a spark discharge atomic emission spectrometer, the conventional instrument can provide two detection results of all aluminum and acid-soluble aluminum according to a built-in algorithm according to the spectrum intensity difference of all aluminum and aluminum oxide.
In conclusion, the accurate detection of the acid-soluble aluminum content in steel is a difficult problem to be solved in the current steel production process, especially in the oriented silicon steel production process.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a method for accurately measuring the content of acid-soluble aluminum in steel, and the sample dissolution temperature and the sample dissolution time in the measuring process of an inductively coupled plasma emission spectrometry are determined according to the reference value of the content of the acid-soluble aluminum detected by a spark discharge atomic emission spectrometer, so that an accurate measuring result of the content of the acid-soluble aluminum is obtained, and the accuracy is controlled within +/-3 ppm.
In order to solve the technical problem, the invention provides a method for accurately measuring the content of acid-soluble aluminum in steel, which comprises the following steps:
1) Taking a block steel sample, placing the block steel sample on an excitation table of a spark discharge atomic emission spectrometer, measuring an acid-soluble aluminum content reference value, and marking the reference value as Als 1 Numerical values are expressed in%;
2) Taking a chip-shaped steel sample, adding a mixed solution of nitric acid and hydrochloric acid, adding perchloric acid after the chip-shaped steel sample is dissolved, heating for dissolving, cooling and fixing the volume to obtain a solution to be measured;
3) And (3) introducing the solution to be measured into an inductively coupled plasma atomic emission spectrometer, and determining the content of the obtained acid-soluble aluminum as an accurate determination result.
In the above scheme, the working conditions of the spark discharge atomic emission spectrometer are as follows: the CCS spark light source is adopted, the analysis gap is 3mm, and the acid-soluble aluminum analysis line is 308.22nm.
In the scheme, the mixed solution of the nitric acid and the hydrochloric acid is formed by mixing the nitric acid and the hydrochloric acid according to the volume ratio of 9:1, wherein the nitric acid is formed by mixing concentrated nitric acid with the density of 1.42g/mL and water according to the volume ratio of 1:3, and the hydrochloric acid is concentrated hydrochloric acid with the density of 1.19 g/mL.
In the above scheme, the density of the perchloric acid is 1.67g/mL.
In the above scheme, the mass of the chip-shaped sample in the step 2) is 0.1-1.0 g, the addition amount of the mixed solution of nitric acid and hydrochloric acid is 3-15 mL, and the addition amount of perchloric acid is 3-10 mL.
In the above-described embodiment, the heating temperature t=als in step 2) 1 ×10 6 +T 1 T in 1 140 to 160, T is in units of ℃.
In the above scheme, the heating time t=als in step 2) 1 ×10 5 +t 1 In t 1 The unit of t is min and is-5 to +5.
In the above scheme, the working conditions of the inductively coupled plasma atomic emission spectrometer are as follows: the rotation speed of the solution leading-in pump is 120-150 rpm, the radio frequency power is 1200-1800W, the observation height is 15-20 mm, the lifting amount of the solution is 0.1-0.6 mL/min, and the light intensity collecting time is 15-30 s.
In the scheme, the content of acid-soluble aluminum in the steel is 0.01-0.04%.
Compared with the prior art, the invention has the beneficial effects that:
according to the initial result of conventional spark discharge atomic emission spectrometry, the invention precisely controls the sample dissolution temperature and sample dissolution time in the measuring process of the inductively coupled plasma emission spectrometry, ensures that acid-soluble elemental aluminum and aluminum nitride are fully dissolved, and simultaneously avoids that small-particle aluminum oxide is partially dissolved in acid by long-time heating at high temperature to influence the accuracy of acid-soluble aluminum detection, so that the accuracy of the final acid-soluble aluminum content detection result is controlled within +/-3 ppm. The accurate measurement of the acid-soluble aluminum content can play an important role in the production of steel, particularly in the production process of oriented silicon steel, the acid-soluble aluminum content is a main basis for making a post-process technology, and the accurate measurement ensures that the technology matching and the magnetic property level reach the expected effect.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrated, but are not limited to the following examples.
In the following examples, the model of the spark discharge atomic emission spectrometer was ARL 4460, and the specific working conditions were: adopting a CCS spark light source, analyzing a gap of 3mm and an acid-soluble aluminum analysis line 308.22nm; before use, the calibration work is completed according to GB/T4336-2016 method for measuring the multi-element content of carbon steel and medium-low alloy steel by using a spark discharge atomic emission spectrometry (conventional method).
In the following examples, the model of the inductively coupled plasma atomic emission spectrometer used was ICAP 7000, and specific working conditions were: the rotation speed of the solution leading-in pump is 150rpm, the radio frequency power is 1600W, the observation height is 18mm, the lifting amount of the solution is 0.4mL/min, and the light intensity acquisition time is 20s; before use, the working curve is drawn according to GB/T20125-2006 "measuring of low alloy steel multielement content inductively coupled plasma emission spectrometry".
In the following embodiment, the mixed solution of nitric acid and hydrochloric acid is formed by mixing nitric acid and hydrochloric acid according to the volume ratio of 9:1, wherein the nitric acid is formed by mixing concentrated nitric acid with the density of 1.42g/mL and water according to the volume ratio of 1:3, and the hydrochloric acid is concentrated hydrochloric acid with the density of 1.19 g/mL; the perchloric acid employed was concentrated perchloric acid having a density of 1.67g/mL.
Examples and comparative examples
Adopting a low-temperature high-magnetic induction oriented silicon steel conventional smelting process to continuously smelt 15 furnaces of steel, taking a steelmaking columnar sample in a tundish in the continuous casting pouring process, and determining the acid-soluble aluminum content in the oriented silicon steel, wherein the method comprises the following steps of:
1) Placing the columnar sample on an excitation table of a spark discharge atomic emission spectrometer, measuring the reference value of the content of acid-soluble aluminum, and marking as Als 1 Numerical values are expressed in%;
2) Preparing a chip sample by drilling or milling a columnar sample, taking the chip sample, adding a mixed solution of nitric acid and hydrochloric acid, adding perchloric acid after the chip sample is dissolved, heating for dissolving, cooling and fixing the volume to obtain a solution to be measured;
3) Introducing the solution to be measured into an inductively coupled plasma atomic emission spectrometer, measuring the content of acid-soluble aluminum, and marking the content as Als, wherein the content is an accurate measurement result;
wherein the heating temperature of each example satisfies t=als 1 ×10 6 +T 1 ，T 1 140 to 160, the heating time satisfies t=als 1 ×10 5 ±5。
Table 1 determination of Process Key parameters
The 15 furnace steel post-working procedures are all used for producing the oriented silicon steel products with the specification of 0.30mm, and the pickling normalizing and decarburization working procedure annealing process is determined according to Als, wherein the normalizing process divides the temperature range by 10ppm according to the Als measured value, and the decarburization process divides the temperature range by 7ppm according to the Als measured value. Evaluating magnetic properties of the finished product, P 17/50 The evaluation is good, the weight of the material is less than or equal to 1.10W/kg; 1.10W/kg < P17/50 Less than or equal to 1.25W/kg, P 17/50 >1.25W/kg was evaluated as waste.
TABLE 2 post process magnetic property level evaluation
As can be seen from Table 2, the final measurement result Als of the method of the present invention and the spark discharge atomic emission spectrometer Als 1 There is a certain difference. When the spark discharge atomic emission spectrometer measures the acid-soluble aluminum content in the oriented silicon steel, the excitation area is a sample micro-area, and when large-particle oxide inclusions, particularly aluminum oxide inclusions exist in the section of the sample to be measured, the measured value of the acid-soluble aluminum is distorted, so that the measurement result of the spark discharge atomic emission spectrometer can only be used as a preliminary estimated value. According to the method, the sample dissolution temperature and the sample dissolution time in the measuring process of the inductively coupled plasma emission spectrometry are determined, so that the acid-soluble aluminum content in the oriented silicon steel is truly and accurately measured. The magnetic property of the finished product finally obtained reaches the expected level by the post-process of the acid-soluble aluminum content formulation measured by the method disclosed by the invention, and the accuracy of the measured value of the method disclosed by the invention is verified. In the comparative example, the sample dissolution temperature and the sample dissolution time do not meet the requirements of the invention, so that the acid-soluble aluminum result is inaccurate, and the magnetic property of the finished product is poor or waste products are generated.
Precision and accuracy test
Taking 3 steel sample standards, and determining the acid-soluble aluminum content in steel, wherein the method comprises the following steps:
1) Since the standard sample is a chip sample, the spark discharge detection cannot be performed, and the known standard value is taken as Als 1 ；
2) Taking 0.5g of chip-shaped standard sample, adding 10mL of mixed solution of nitric acid and hydrochloric acid, adding 5mL of perchloric acid after the standard sample is dissolved, heating for dissolving, cooling and fixing the volume to obtain a solution to be measured;
3) And (3) introducing the solution to be measured into an inductively coupled plasma atomic emission spectrometer, and measuring the content of acid-soluble aluminum, namely Als.
Table 3 standard measurement parameters and results
As can be seen from Table 3, if the heating temperature and the heating time are not controlled, the too high heating temperature or the too long heating time may cause the small-particle aluminum oxide to be dissolved in the acid so as to cause the detection result to be relatively high, and the too low heating temperature or the too short heating time may cause the large-particle aluminum nitride to be not timely dissolved in the acid so as to cause the detection result to be relatively low, the heating temperature and the heating time are strictly controlled, so that the accurate measurement result of the acid-soluble aluminum content is obtained, and the accuracy is controlled within +/-3 ppm.
The above examples are presented for clarity of illustration only and are not limiting of the embodiments. Other variations or modifications of the above description will be apparent to those of ordinary skill in the art, and it is not necessary or exhaustive of all embodiments, and thus all obvious variations or modifications that come within the scope of the invention are desired to be protected.
Claims (6)
1. The method for precisely measuring the content of the acid-soluble aluminum in the steel is characterized by comprising the following steps of:
1) Taking a block steel sample, placing the block steel sample on an excitation table of a spark discharge atomic emission spectrometer, measuring an acid-soluble aluminum content reference value, and marking the reference value as Als 1 Numerical values are expressed in%;
2) Taking a chip-shaped steel sample, adding a mixed solution of nitric acid and hydrochloric acid, adding perchloric acid after the chip-shaped steel sample is dissolved, heating for dissolving, cooling and fixing the volume to obtain a solution to be measured; wherein the heating temperature t=als 1 ×10 6 +T 1 Unit of temperature, T 1 140 to 160; heating time t=als 1 ×10 5 +t 1 Units min, t 1 Is-5 to +5;
3) And (3) introducing the solution to be measured into an inductively coupled plasma atomic emission spectrometer, and determining the content of the obtained acid-soluble aluminum as an accurate determination result.
2. The method for precisely measuring the content of acid-soluble aluminum in steel according to claim 1, wherein the mass of the chip-like sample in the step 2) is 0.1-1.0 g, the addition amount of the mixed solution of nitric acid and hydrochloric acid is 3-15 mL, and the addition amount of perchloric acid is 3-10 mL.
3. The method for precisely determining the acid-soluble aluminum content in steel according to claim 1 or 2, wherein the mixed solution of nitric acid and hydrochloric acid is formed by mixing nitric acid and hydrochloric acid according to a volume ratio of 9:1, wherein the nitric acid is formed by mixing concentrated nitric acid with a density of 1.42g/mL and water according to a volume ratio of 1:3, and the hydrochloric acid is concentrated hydrochloric acid with a density of 1.19 g/mL; the density of the perchloric acid is 1.67g/mL.
4. The method for precisely determining the content of acid-soluble aluminum in steel according to claim 1, wherein the content of acid-soluble aluminum in the steel is 0.01-0.04%.
5. The method for precisely determining the content of acid-soluble aluminum in steel according to claim 1, wherein the working conditions of the spark discharge atomic emission spectrometer are as follows: the CCS spark light source is adopted, the analysis gap is 3mm, and the acid-soluble aluminum analysis line is 308.22nm.
6. The method for precisely determining the content of acid-soluble aluminum in steel according to claim 1, wherein the working conditions of the inductively coupled plasma atomic emission spectrometer are as follows: the rotation speed of the solution leading-in pump is 120-150 rpm, the radio frequency power is 1200-1800W, the observation height is 15-20 mm, the lifting amount of the solution is 0.1-0.6 mL/min, and the light intensity collecting time is 15-30 s.
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