Element measurement method based on dual-spectrum fusion

Abstract

The invention belongs to the technical field of spectrums, and particularly relates to an element measurement method based on double-spectrum fusion, which comprises the following steps: acquiring the spectral intensity X1i of a first type of elements B1i by using an XRF (X-Ray Fluorescence) technology, acquiring the spectral intensity L1i of the first type of elements B1i and the spectral intensity L2j of a second type of elements B2j by using an LIBS (Laser-induced Breakdown Spectroscopy) technology, i = 1, 2... M, j = 1, 2... N, and M and N are integers not less than 2; correcting the spectral intensity X1i into X1i '; obtaining a correction function g (X1k ' / L1k) by using the correction spectral intensities X1k'and L1k of the element B1k; the spectral intensity L2j is corrected to L2j '= L2j.g (X1k' / L1k); and obtaining the content C1i of the first type of elements B1i according to the X1i ', and obtaining the content C2j of the second type of elements B2j according to the L2j'. The method has the advantages of high measurement precision and the like.

Description

Technical Field

[0001] The present invention relates to the field of spectral technology, and particularly to an element measurement method based on dual-spectrum fusion. Background Art

[0002] LIBS is an advanced atomic emission spectroscopy technology. However, there are many factors affecting the intensity of the measured spectrum, such as the energy of the laser, the size of the converging light spot, the particle size of the measured object, etc. These influencing factors will ultimately lead to a decrease in the accuracy of measuring the element content by LIBS.

[0003] The XRF technology is a rapid and non-destructive material measurement method. Specifically, a high-energy X-ray is used to bombard the material, and the material emits a fluorescence signal, which is converted into an electrical signal by a fluorescence signal detector. The XRF technology has advantages such as high sensitivity and high precision in detecting high-quality elements, but it has insufficient precision in detecting low-quality elements. Summary of the Invention

[0004] To solve the deficiencies in the above prior art solutions, the present invention provides an element measurement method based on dual-spectrum fusion.

[0005] The object of the present invention is achieved by the following technical solutions: An element measurement method based on dual-spectrum fusion, comprising the following steps: Obtain the spectral intensity X of the first type of element B using XRF technology 1i of 1i , obtain the spectral intensity L of the first type of element B using LIBS technology 1i and the spectral intensity L of the second type of element B 1i , i = 1, 2 ··· M, j = 1, 2 ··· N, where both M and N are integers not less than 2; 2j of 2j ; The spectral intensity X 1i is corrected to X 1i ˊ = X 1i · f(D, R), where f(D, R) is a correction function, D is the distance between the X-ray light source reference plane and the measured object, and R is the average particle size of the measured object; Utilize the corrected spectral intensity X of element B 1k to obtain the correction function g(X 1k ˊ / L 1k ); 1k ˊ / L 1k ) The spectral intensity L 2j is corrected to L 2j ˊ = L2j ·g(X 1k ˊ / L 1k ); Obtain the content C of the first type of element B according to X 1i ˊ and obtain the content C of the second type of element B according to L 1i . 1i 2j ˊ 2j . 2j

[0006] Compared with the prior art, the beneficial effects of the present invention are as follows: Integrate the advantages of LIBS technology and XRF technology, and use high-precision XRF spectra to dynamically compensate LIBS spectra. For example, use the spectra of elements with high signal-to-noise ratio and good linearity to compensate the LIBS spectra of low-quality elements, thereby significantly improving the detection accuracy of low-quality elements; Use the correction function f(D, R) to compensate for the influence of distance and the particle size of the measured object, improve the detection accuracy, and thus achieve high-precision measurement of all elements. BRIEF DESCRIPTION OF THE DRAWINGS

[0007] Referring to the accompanying drawings, the disclosure of the present invention will become more understandable. It is easy for those skilled in the art to understand that these drawings are only used to illustrate the technical solutions of the present invention and are not intended to limit the protection scope of the present invention. In the drawings: Figure 1 is a schematic flow chart of the element measurement method based on dual-spectrum fusion of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0008] Figure 1 The following description and illustration describe alternative specific embodiments of the present invention to teach those skilled in the art how to implement and reproduce the present invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the technical solutions of the present invention. Those skilled in the art should understand that variations or substitutions derived from these specific embodiments will fall within the scope of the present invention. Those skilled in the art should understand that the following features can be combined in various ways to form multiple variations of the present invention. Thus, the present invention is not limited to the following alternative specific embodiments, but is defined only by the claims and their equivalents.

[0009] Example 1:

[0010] A method for measuring elements based on dual-spectrum fusion in this embodiment, as Figure 1 shown, the measurement method includes the following steps: Use XRF technology to obtain the spectral intensity X of the first type of element B 1i 1i ​​​, the first type of element B is obtained using LIBS technology 1i Spectral intensity L 1i and the second type of element B 2j spectral intensity L 2j , where i = 1, 2 ··· M, j = 1, 2 ··· N, and both M and N are integers not less than 2; Spectral intensity X 1i is corrected to X 1i ˊ = X 1i · f(D, R), where f(D, R) is a correction function, D is the distance between the X-ray light source reference plane and the object to be measured, and R is the average particle size of the object to be measured; Using the corrected spectral intensity X 1k of element B 1k ˊ and L 1k to obtain the correction function g(X 1k ˊ / L 1k ), and element B 1k should meet the requirements of high signal-to-noise ratio and good linearity.

[0011] Spectral intensity L 2j is corrected to L 2j ˊ = L 2j · g(X 1k ˊ / L 1k ); According to X 1i ˊ to obtain the content C 1i of the first type of element B 1i , and according to L 2j ˊ to obtain the content C 2j of the second type of element B 2j .

[0012] To give full play to the respective advantages of XRF technology and LIBS technology, further, the first type of element is an element with an atomic number greater than 12, such as iron, copper, and calcium, and the second type of element is an element with an atomic number less than 12, such as carbon, oxygen, and sodium, and the element B 1k is iron.

[0013] To obtain the content of each element, C 1i = K 1i · X 1i ˊ + b 1i , C 2j = K 2j · L 2j ˊ + b 2j, K 1i , b 1i are the coefficients corresponding to the first type of element B 1i respectively. K 2j , b 2j are the coefficients corresponding to the second type of element B 2j respectively.

[0014] Example 2:

[0015] According to the application example of the measurement method in Embodiment 1 of the present invention, it is used to measure the contents of calcium, iron, copper, carbon, oxygen, and sodium elements in the object to be measured.

[0016] In this application example, as Figure 1 shown, the measurement method includes the following steps: Using XRF technology to measure the first type of elements, such as elements like calcium, iron, and copper (element numbers greater than 12), which have relatively strong X-ray fluorescence spectrum signals, respectively: For iron element, the characteristic fluorescence energy is 6.403 keV, and the spectrum intensity X 11 is 52060 (counts).

[0017] For copper element, the characteristic fluorescence energy is 8.047 keV, and the spectrum intensity X 12 is 13840 (counts).

[0018] For calcium element, the characteristic fluorescence energy is 3.69 keV, and the spectrum intensity X 13 is 1200 (counts).

[0019] Using LIBS technology to obtain the atomic emission spectrum signals of the first type of elements (calcium, iron, copper) and the second type of elements (carbon, oxygen, sodium), respectively: The LIBS intensity L of iron element 11 is 6290 (counts).

[0020] The LIBS intensity L of copper element 12 is 1550 (counts).

[0021] The LIBS intensity L of calcium element 13 is 980 (counts).

[0022] For carbon element, the LIBS intensity L 21 is 2160 (counts).

[0023] For oxygen element, the LIBS intensity L 22 is 3740 (counts).

[0024] For sodium element, the LIBS intensity L 23is 610 (counts).

[0025] The ranging unit obtains the distance D = 13 mm from the reference plane of the X-ray light source to the object to be measured, and the particle size measuring unit obtains the average particle size R = 4.7 mm of the object to be measured.

[0026] The correction function f(D, R) = 0.0005·D 2 - 0.001·R 2 + 0.01·D + 0.02·R - 0.0005·D·R + 0.9407.

[0027] When the XRF technology measures calcium, copper, and iron elements, with a distance D = 13 mm and an average particle size R = 4.7 mm, f(D, R) is approximately 1.1966, and the correction of the spectral intensity of the first type of elements is obtained: The corrected intensity X of the iron element 11 ˊ = X 11 ·f(D, R) = 62295.41 (counts).

[0028] The corrected intensity X of the copper element 12 ˊ = X 12 ·f(D, R) = 16561.05 (counts).

[0029] The corrected intensity X of the calcium element 13 ˊ = X 13 ·f(D, R) = 1435.9 (counts).

[0030] Select the iron element with high signal-to-noise ratio and good linearity as the characteristic element B 11 , and use the corrected spectral intensity X 11 ˊ 、X 11 to obtain the correction function g(X 11 ˊ / L 11 ).

[0031] g(X 11 ˊ / L 11 ) = 0.003(X 11 ˊ / L 11 ) 3 - 0.008(X 11 ˊ / L 11 ) 2 + 0.08(X 11 ˊ / L 11) + 1.05。

[0032] Use the correction function to correct the spectral intensities of carbon, oxygen, and sodium elements: The spectral intensity of carbon element L 21 Is corrected to L 21 ˊ = L 21 · g(X 11 ˊ / L 11 ) = 2913.94 (counts).

[0033] The spectral intensity of oxygen element L 22 Is corrected to L 22 ˊ = L 22 · g(X 11 ˊ / L 11 ) = 5045.44 (counts).

[0034] The spectral intensity of sodium element L 23 Is corrected to L 23 ˊ = L 23 · g(X 11 ˊ / L 11 ) = 822.92 (counts).

[0035] For carbon, oxygen, and sodium elements with atomic numbers less than 12, use the corrected spectral intensity L 2j ˊ To perform the inversion calculation of concentration, and for calcium, iron, and copper elements with atomic numbers greater than 12, use the corrected spectral intensity X 1i ˊ To perform the inversion calculation of concentration.

[0036] The iron content C 11 = 0.000416 · X 11 ˊ - 0.025 = 25.88 (wt%).

[0037] The copper content C 12 = 0.00107 · X 12 ˊ - 0.946 = 16.77 (wt%).

[0038] The calcium content C 13 = 0.00208 · X 13 ˊ - 0.483 = 2.50 (wt%).

[0039] The carbon content C 21=0.00264·L 21 ˊ -0.297 = 7.40 (wt%)。

[0040] Oxygen content C 22 =0.00831·L 22 ˊ -2.084 = 39.84 (wt%)。

[0041] Sodium content C 23 =0.00595·L 23 ˊ -0.5484 = 4.35 (wt%)。

Claims

1. An element measurement method based on dual-spectrum fusion, characterized in that, The described element measurement method includes the following steps: Obtain the spectral intensity X of the first type of element B using XRF technology 1i and obtain the spectral intensity L of the first type of element B using LIBS technology 1i and the spectral intensity L of the second type of element B 1i where i = 1, 2 ··· M, j = 1, 2 ··· N, and both M and N are integers not less than 2 1i 2j 2j ​​​ Spectral intensity X 1i Corrected to X 1i ˊ =X 1i ·f(D, R), where f(D, R) is a correction function, D is the distance between the reference plane of the X-ray light source and the object to be measured, and R is the average particle size of the object to be measured; Using element B 1k The corrected spectral intensity X 1k ˊ and L 1k to obtain the correction function g(X 1k ˊ / L 1k ); Spectral intensity L 2j Modified to L 2j ˊ = L 2j ·g(X 1k ˊ / L 1k ); According to X 1i ˊ obtain the content C of the first type of element B 1i of 1i According to L 2j ˊ obtain the content C of the second type of element B 2j of 2j .

2. The elemental measurement method based on dual-spectrum fusion according to claim 1, wherein The first type of elements are elements with an atomic number greater than 12, and the second type of elements are elements with an atomic number less than 12.

3. The elemental measurement method based on dual-spectrum fusion according to claim 2, wherein The first type of elements includes iron, copper and calcium, and the second type of elements includes carbon, oxygen and sodium, and the element B 1k is iron.

4. The element measurement method based on dual-spectrum fusion according to claim 1, characterized in that C 1i =K 1i ·X 1i ˊ +b 1i ,C 2j =K 2j ·L 2j ˊ +b 2j ,K 1i 、b 1i are respectively the coefficients corresponding to the first type of element B 1i ,K 2j 、b 2j are respectively the coefficients corresponding to the second type of element B 2j .

5. The elemental measurement method based on dual-spectrum fusion according to claim 4, wherein, The first type of element B 1i The contents are respectively: Iron content C 11 = 0.000416·X 11 ˊ -0.025, copper content C 12 = 0.00107·X 12 ˊ -0.946, calcium content C 13 = 0.00208·X 13 ˊ -0.483; The second type of element B 2j The contents are respectively: Carbon content C 21 = 0.00264·L 21 ˊ -0.297, oxygen content C 22 = 0.00831·L 22 ˊ -2.084, sodium content C 23 = 0.00595·L 23 ˊ -0.5484 6. The element measurement method based on dual-spectrum fusion according to claim 1, characterized in that g(X 1k ˊ / L 1k ) = 0.003(X 1k ˊ / L 1k ) 3 - 0.008(X 1k ˊ / L 1k ) 2 + 0.08(X 1k ˊ / L 1k ) + 1.05。 7. The element measurement method based on dual-spectrum fusion according to claim 1, characterized in that f(D,R)=0.0005·D 2 -0.001·R 2 +0.01·D+0.02·R-0.0005·D·R+0.9407。

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