CN115954070B - Correction method for diffraction intensity of high-angle X-ray twin diffraction point - Google Patents
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- 238000012937 correction Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000011159 matrix material Substances 0.000 claims abstract description 17
- 238000004364 calculation method Methods 0.000 claims abstract description 12
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- 239000011733 molybdenum Substances 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims description 11
- 238000002474 experimental method Methods 0.000 claims description 7
- 239000013598 vector Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 13
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000010586 diagram Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000001149 cognitive effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
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- 230000003068 static effect Effects 0.000 description 1
- 230000005428 wave function Effects 0.000 description 1
Abstract
The invention belongs to the field of material subdivision, and discloses a method for correcting diffraction intensity of a high-angle X-ray twin diffraction point, which comprises the following steps: step one, an X-ray source of a molybdenum target, the presence ofAndtwo adjacent diffraction points with different intensities are generated by diffraction of light with two wavelengths, and a diffraction point P with large intensity is obtained 1 Calculating an orientation matrix of the diffraction point; step two: according to the orientation matrix and P 1 Position calculation of diffraction Point and P 1 Corresponding P 2 The location of the diffraction point; step three: p pair P 1 And P 2 The diffraction points are integrated to calculate the intensity I (P) 1 ) And I (P) 2 ) The corrected intensity is I Correction of ＝I(P 1 )+I(P 2 ). Compared with the prior art, the invention has the beneficial effects that: by integrating the intensities of two separate diffraction points of each coordinate system K (h, K, l) separately, an accurate I is obtained Correction of (h, k, l), corrected I Correction of (h, k, l) is more conducive to accuracy of electronic structure refinement.
Description
Technical Field
The invention relates to the technical field of material analysis, in particular to a method for correcting diffraction intensity of a high-angle X-ray twin diffraction point of an X-ray diffraction experiment.
Background
Material science is the basis and guide of modern science and technology, and the cognitive level of material structure and material construction relationship directly determines the research and development capability of new materials.
The microstructure of the material comprises an atomic layer structure such as a crystal structure, a local structure, a defect structure and the like and an electronic structure, wherein the electronic structure fundamentally determines the intrinsic performance of the material. At present, experimental testing technology of a material atomic hierarchy structure has been developed very mature, but experimental testing of an electronic structure is always in an exploration stage, and although the electronic structure can be obtained by first theoretical calculation, the theoretical calculation adopts a plurality of assumptions, the calculation result is deviated from the actual situation, and the design of a high-performance material is difficult to guide.
Thus, how to obtain experimental electronic structures of materials is a key scientific issue. The solution of the problem is helpful for realizing the spanning from atomic level to electronic level of experimental study of the material structure in China, and accelerating the research and development process of a batch of national defense and civil key functional materials.
Fig. 1 is a diagram showing an experimental structure of the prior art using X-rays, the X-rays are incident on a crystal to be tested, the X-rays are diffracted after passing through the crystal to be tested, high-precision and high-resolution X-ray single crystal diffraction data (position and intensity information) can be obtained through an X-ray detector, and an electronic structure refinement is performed, so that an experimental electronic structure of a material can be reversely deduced, and finally, an experimental electronic structure of the material under static and active conditions can be obtained, wherein the electronic structure can be described by using an electron density, a density matrix or an electron wave function.
As shown in FIG. 1a, X-rays are irradiated on the crystal, because atoms in the crystal are orderly arranged, the X-rays are diffracted to form innumerable diffraction spots, each diffraction spot can be represented by three integers h, K and l, three directions corresponding to three-dimensional space respectively are selected, spots K (h, K and l) in the diffraction spots are selected,
as shown in fig. 2a,2 b: in the X-ray diffraction experiment process, if a molybdenum target X-ray source is used, the X-ray source is not monochromatic light and existsAnd->Light of both wavelengths has many twinning diffraction points which give errors in the final result, as shown in fig. 2 b.
Disclosure of Invention
The invention provides a method for correcting diffraction intensity of a high-angle X-ray twin diffraction point.
In order to achieve the above purpose, the present invention adopts the following technical scheme: a method of correcting diffraction intensity of a high angle X-ray twin diffraction point, comprising: step one, an X-ray source of a molybdenum target, the presence ofAndtwo adjacent diffraction points with different intensities are generated by diffraction of light with two wavelengths, and diffraction point k with high intensity is obtained α1 Calculates the position of the (b)Orientation matrix of diffraction points->Step two: according to the orientation matrix and P 1 Position calculation of diffraction Point and P 1 Corresponding P 2 The location of the diffraction point; step three: p pair P 1 And P 2 The diffraction points are integrated to calculate the intensity I (P) 1 ) And I (P) 2 ) The corrected intensity is I Correction of ＝I(P 1 )+I(P 2 ) The method comprises the steps of carrying out a first treatment on the surface of the Step three: p pair P 1 And P 2 The diffraction points are integrated to calculate the intensity I (P) 1 ) And I (P) 2 ) The corrected intensity is I Correction of ＝I(P 1 )+I(P 2 )。
Wherein, the preferable scheme is as follows: in the first step, two adjacent diffraction points appear at any point K (h, K, l) in the coordinate system, which is defined as: p (P) 1 (x 1 ,y 1 ,z 1 ) And P 2 (x 2 ,y 2 ,z 2 )，P 1 And P 2 Diffraction points, P, respectively corresponding to kα1 and kα2 1 Is greater than P 2 Is obtained by diffraction experiment 1 (x 1 ,y 1 ,z 1 ) The orientation matrix of the crystal can be obtained through index calculation
Wherein, the preferable scheme is as follows: the P is 1 Is greater than P 2 Twice the intensity of (a).
Wherein, the preferable scheme is as follows: in the second step, due to P 1 Diffraction point and P 2 The diffraction points have the same orientation matrix U, according to U andand +.>Calculating P 2 Precise position P of diffraction point 2 (x 2 ,y 2 ,z 2 )。
Wherein, the preferable scheme is as follows: step three, P of coordinate system K (h, K, l) 1 And P 2 The diffraction points are integrated to calculate the intensity I (P) 1 ) And I (P) 2 ) The corrected intensity is I Correction of (h，k，l)＝I(P 1 )+I(P 2 )。
Wherein, the preferable scheme is as follows: use I Correction of (h, k, l) is incorporated into the electronic structure refinement.
Compared with the prior art, the invention has the beneficial effects that: by integrating the intensities of two separate diffraction points of each coordinate system K (h, K, l) separately, an accurate I is obtained Correction of (h, k, l), corrected I Correction of (h, k, l) is more conducive to accuracy of electronic structure refinement.
Drawings
FIG. 1 is a diagram showing an experimental structure of the prior art using X-rays;
FIG. 1a is a block diagram of a prior art diffraction spot displayed at low angles using a molybdenum target X-ray source;
FIGS. 2a,2b are block diagrams of twinning diffraction spots displayed at high angles using a molybdenum target X-ray source in the prior art;
FIG. 3 is a flow chart of a method of correcting diffraction intensity of a high angle X-ray twinning diffraction point according to the present invention;
FIG. 4 is a schematic diagram of a method for correcting diffraction intensity of a high-angle X-ray twinning diffraction point according to the present invention;
FIG. 5 is a schematic diagram of the index calculation of diffraction intensity of the high-angle X-ray twin diffraction point of the present invention;
FIG. 6 is a schematic representation of an equidistant three-dimensional grid definition of diffraction intensity for a high angle X-ray twinning diffraction spot of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
As shown in fig. 3 and 4: to obtain more accurate I by correction Correction of (h，k，l)。
Comprising the following steps: step one, using a molybdenum target X-ray source, in the presence ofAndlight of two wavelengths, at high angles, each k (h, k, l) diffraction point will appear as two adjacent diffraction points, denoted as P 1 (x 1 ,y 1 ,z 1 ) And P 2 (x 2 ,y 2 ,z 2 )，P 1 And P 2 Respectively corresponding to k α1 And k α2 Diffraction point, P of the generation 1 Is greater than P 2 Is obtained by diffraction experiment 1 (x 1 ,y 1 ,z 1 ) By indexing calculation, i.e. drawing a set of equidistant three-dimensional grids, wherein the smallest grid is a parallelepiped, as shown in fig. 5 and 6: let all P 1 (x 1 ,y 1 ,z 1 ) Are all just above the lattice points of the lattice, a matrix describing the minimum parallelepiped size and orientation (orientation matrix for short) is obtained>One crystal has a unique orientation matrix. And all the lattice points are represented by indexes (h, k, l) represented by a set of three integers, the center-most lattice point is marked as (0 0 0), the lattice points along the x direction of the three-dimensional space are marked as (1 0), (2 0 0), (3 0) …, etc. in turn, the lattice points along the y direction are marked as (0 1 0), (0 2 0), (0 3 0) …, etc. and the lattice points along the z direction are marked as (0 1), (0 2), (0 3) …, etc. in turn; step two, due to P 1 Diffraction point and P 2 Diffraction spots are from the same crystal and have the same orientation matrix U, according to U and +.>AndCalculating the accurate position P2 (x) 2 ,y 2 ,z 2 )；
Step three, P for the spot position coordinates K (h, K, l) 1 And P 2 The diffraction points are integrated to calculate the intensity I (P) 1 ) And I (P) 2 ) The corrected intensity is I Correction of ＝I(P 1 )+I(P 2 )。
How to pass P 1 (x 1 ,y 1 ,z 1 ) And P 2 (x 2 ,y 2 ,z 2 ) Under the condition of corresponding to index position K (h, K, l), obtaining a set of relatively strong P through diffraction experiment 1 (x 1 ,y 1 ,z 1 ) Comprising n (n is typically thousands or tens of thousands) diffraction points P 1 1 (x 1 1 ,y 1 1 ,z 1 1 ),P 1 2 (x 1 2 ,y 1 2 ,z 1 2 ),
P 1 3 (x 1 3 ,y 1 3 ,z 1 3 ),…,P 1 n (x 1 n ,y 1 n ,z 1 n ) Wherein x is 1 ,y 1 ,z 1 The center coordinates of each diffraction point are respectively calculated as P, and index positions K (h, K, l) of each diffraction point can be obtained through indexing 1 1 (h 1 ,k 1 ,l 1 ),P 1 2 (h 2 ,k 2 ,l 2 ),P 1 3 (h 3 ,k 3 ,l 3 ),…,P 1 n (h n ,k n ,l n ),P 2 (x 2 ,y 2 ,z 2 ) And P 1 (x 1 ,y 1 ,z 1 ) The two sets of data are identical. And further from P 1 (x 1 ,y 1 ,z 1 ) The relation with K (h, K, l) is:
wherein λ1= 0.7093, n equations can be established by using P1 data according to the equation, and least square iterative calculation is performed to obtain the optimal +.>
Taking a well-known nonlinear optical crystal AgGaS2 as an example, diffraction points are tested, and electron densities refined under the two conditions of correction and non-correction according to the method are measured:
table 1 shows the spot center position P obtained by AgGaS2 experiments 1 (x 1 ,y 1 ,z 1 ) And the corresponding K (h, K, l) index
It can be easily inferred from Table 1 that P 1 Orientation matrix of (2) is In this embodiment, a= (-0.006881,0.006735, -0.096694); b= (-0.000344, -0.174046, -0.003785); c= (-0.174058, -0.000020,0.003743), x= (1, 0), y= (0, 1, 0), z= (0, 1).
Due to P 2 Diffraction point and P 1 The diffraction spots have the same orientation matrix U, known U andandCalculating P 2 Precise position P of diffraction point 2 (x 2 ,y 2 ,z 2 ) The method comprises the steps of carrying out a first treatment on the surface of the As shown in table 2:
table 2 shows P at the AgGaS2 position index parameter K (h, K, l) 2 (x 2 ,y 2 ,z 2 ) Value of
P for a blob of the blob coordinate position parameter (h, k, l) 1 And P 2 The diffraction points are integrated to calculate the intensity I (P) 1 )、I(P 2 ) The corrected intensity is I Correction of (h，k，l)＝I(P 1 )+I(P 2 ) As shown in Table 3, finally use I Correction of (h, k, l) performing electronic structure refinement.
Table 3 shows I under the AgGaS2 position index parameter K (h, K, l) Without correction ，I(P 1 )，I(P 2 ) Value and I Correction of 。
The comparison is made by the first performance calculation and the results of the AGS sample test of table 4, the results corrected by the scheme of this patent are closer to the theoretical value, and the results not corrected are far from the theoretical value, indicating that the scheme of this patent is feasible.
Table 4 shows the AGS sample calibration before and after comparison
Compared with the prior art, the invention has the beneficial effects that: by integrating the intensities of two discrete diffraction points of the three-dimensional extension index K (h, K, l) of the spot respectively, an accurate I is obtained Correction of (h, k, l), corrected I Correction of (h, k, l) is more conducive to accuracy of electronic structure refinement.
Claims (4)
1. A method for correcting diffraction intensity of a high-angle X-ray twin diffraction point is characterized by comprising the following steps of: step one, an X-ray source of a molybdenum target, the presence ofAnd k α2 />Two adjacent diffraction points with different intensities are generated by diffraction of light with two wavelengths, and a diffraction point P with large intensity is obtained 1 Is used for calculating the orientation matrix of the diffraction pointStep two: according to the orientation matrix and P 1 Position calculation of diffraction Point and P 1 Corresponding P 2 The position of the diffraction point due to P 1 Diffraction point and P 2 The diffraction points have the same orientation matrix U, according to U andand +.>Calculating P 2 Precise position P of diffraction point 2 (x 2 ,y 2 ,z 2 ) The method comprises the steps of carrying out a first treatment on the surface of the Step three: p under position index parameter K (h, K, l) 1 And P 2 The diffraction points are integrated to calculate the intensity I (P) 1 ) And I (P) 2 ) The corrected intensity is I Correction of ＝I(P 1 )+I(P 2 )。
2. The method for correcting the diffraction intensity of the high-angle X-ray twin diffraction point according to claim 1, wherein: in the first step, two adjacent diffraction points with the same index K (h, K, l) are selected, and are defined as: p (P) 1 (x 1 ,y 1 ,z 1 ) And P 2 (x 2 ,y 2 ,z 2 ) They respectively represent P 1 、P 2 Position in rectangular coordinate system of detecting instrument, P 1 And P 2 Respectively corresponding to k α1 And k α2 Diffraction point, P of the generation 1 Is greater than P 2 Is obtained by diffraction experiment 1 (x 1 ,y 1 ,z 1 ) The orientation matrix of the crystal can be obtained through index calculationWherein a, b and c are respectively three axis vectors of the parallelepiped.
3. The method for correcting the diffraction intensity of the high-angle X-ray twin diffraction point according to claim 2, characterized in that: the P is 1 Is greater than P 2 Twice the intensity of (a).
4. The method for correcting the diffraction intensity of the high-angle X-ray twin diffraction point according to claim 1, wherein: use I Correction of (h, k, l) is incorporated into the electronic structure refinement.
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