CN220188400U - X-ray diffraction and X-ray fluorescence spectrum synchronous combination system and device - Google Patents
X-ray diffraction and X-ray fluorescence spectrum synchronous combination system and device Download PDFInfo
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- CN220188400U CN220188400U CN202320588853.6U CN202320588853U CN220188400U CN 220188400 U CN220188400 U CN 220188400U CN 202320588853 U CN202320588853 U CN 202320588853U CN 220188400 U CN220188400 U CN 220188400U
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- 238000002441 X-ray diffraction Methods 0.000 title claims abstract description 98
- 238000004876 x-ray fluorescence Methods 0.000 title claims abstract description 35
- 238000001228 spectrum Methods 0.000 title claims abstract description 34
- 230000001360 synchronised effect Effects 0.000 title claims abstract description 31
- 238000001514 detection method Methods 0.000 claims abstract description 45
- 238000002189 fluorescence spectrum Methods 0.000 claims abstract description 21
- 230000005540 biological transmission Effects 0.000 claims abstract description 10
- 238000004846 x-ray emission Methods 0.000 claims description 66
- 239000000203 mixture Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- 238000012360 testing method Methods 0.000 abstract description 8
- 230000003287 optical effect Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 56
- 239000000126 substance Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 238000010146 3D printing Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000012863 analytical testing Methods 0.000 description 1
- -1 block Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
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- 238000007689 inspection Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000002186 photoelectron spectrum Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
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Abstract
The utility model discloses a synchronous combination system and device of X-ray diffraction and X-ray fluorescence spectrum, and relates to the technical field of X-rays; placing a sample to be tested on a sample table; the synchronous combination system emits X rays to a sample to be detected through an X ray light source subsystem; diffracting X-rays by a sample to be detected to form a diffraction signal; exciting a sample to be detected by X rays to form a fluorescent signal; the XRF detection subsystem is connected with the computer, and obtains a fluorescence spectrum according to the fluorescence signal; the XRD detection subsystem is connected with the computer and is arranged on a transmission optical path of the diffraction signal, and an X-ray diffraction result is obtained by the XRD detection subsystem according to the diffraction signal; the utility model realizes the synchronous test of XRD diffraction and XRF fluorescence spectrum at the same position of the sample to be tested.
Description
Technical Field
The utility model relates to the technical field of X rays, in particular to a synchronous combination device of X-ray diffraction and X-ray fluorescence spectrum.
Background
X-rays are electromagnetic waves having a wavelength in the range of 0.01-10mm, and methods such as X-ray absorption spectrum, fluorescence spectrum, photoelectron spectrum, scattering and diffraction have been developed by utilizing the interaction between X-rays and substances. Wherein X-ray diffraction (XRD) is to precisely measure the crystal structure, texture and stress of a substance by diffracting an X-ray after irradiating the crystal having a periodic structure; x-ray fluorescence spectroscopy (XRF) is a principle that uses different elements to absorb X-rays and then emit fluorescence (X-rays) of different energies to qualitatively or quantitatively determine the elemental composition of a substance. The two methods are widely used in aspects of scientific research, inspection and detection, quality control of products by enterprises and the like.
Typically, both methods are tested using separate instruments, an X-ray diffractometer and an X-ray fluorescence spectrometer, respectively. XRD can obtain X-ray results to analyze the species and crystal phases of the substance, but the diffraction data of the same species, which are often similar in element composition, are quite close and are difficult to distinguish. XRF can obtain an X-ray fluorescence spectrum to analyze the elemental composition of a substance, but the valence of an element, i.e., the crystalline phase of the substance, cannot be known. Therefore, these two methods are generally used together, and the composition of the substances can be more easily resolved through mutual verification, so that many analytical testing departments need to be equipped with two instruments.
However, in the prior art, the two methods are mainly used for independent test to obtain results for analysis, so that the efficiency is low, and an instrument for synchronously combining X-ray diffraction and X-ray fluorescence spectrum is needed.
Disclosure of Invention
The utility model aims to provide an X-ray diffraction and X-ray fluorescence spectrum synchronous combination system and device, which realize synchronous testing of XRD diffraction and XRF fluorescence spectrum at the same position of a sample to be tested.
In order to achieve the above object, the present utility model provides the following solutions:
an X-ray diffraction and X-ray fluorescence spectrum synchronous combination system; placing a sample to be tested on a sample table; the X-ray diffraction and X-ray fluorescence spectrum synchronous combination system comprises:
an X-ray light source subsystem for emitting X-rays to the sample to be measured; the sample to be tested diffracts the X-rays to form diffraction signals; exciting the sample to be detected by the X-rays to form a fluorescent signal;
the XRF detection subsystem is arranged on the sample platform and is used for obtaining a fluorescence spectrum according to the fluorescence signal; the sample stage is arranged on a transmission light path of the X-rays;
the XRD detection subsystem is arranged on a transmission light path of the diffraction signal and used for obtaining an X-ray diffraction result according to the diffraction signal.
Optionally, the X-ray light source subsystem comprises:
an X-ray light source emitter for emitting X-rays to the sample to be measured;
and the X-ray light source bracket is used for fixing the X-ray light source emitter.
Optionally, the XRF detection subsystem comprises:
an XRF detector for obtaining a fluorescence spectrum from the fluorescence signal;
and the XRF detector bracket is arranged on the sample platform and used for fixing the XRF detector.
Optionally, the XRF detector is a Si-PIN detector or an SDD detector.
Optionally, the XRD detection subsystem comprises:
the XRD detector is arranged on a transmission light path of the diffraction signal and is used for obtaining an X-ray diffraction result according to the diffraction signal;
and the XRD detector bracket is used for fixing the XRD detector.
Optionally, the XRD detector is a one-dimensional array detector or a two-dimensional array detector.
Optionally, the system for synchronously combining X-ray diffraction and X-ray fluorescence spectrum further comprises:
and the safety shell is internally provided with the X-ray light source subsystem, the XRF detection subsystem and the XRD detection subsystem.
In order to achieve the above purpose, the present utility model also provides the following solutions:
an X-ray diffraction and X-ray fluorescence spectrum synchrony combination device, the X-ray diffraction and X-ray fluorescence spectrum synchrony combination device comprising:
the system for synchronously combining the X-ray diffraction and the X-ray fluorescence spectrum;
the sample stage is used for placing a sample to be tested; the XRF detection subsystem of the synchronous combination system of X-ray diffraction and X-ray fluorescence spectrum is arranged on the sample table; the X-ray light source subsystem of the X-ray diffraction and X-ray fluorescence spectrum synchronous combination system is used for emitting X-rays to the sample to be detected on the sample table; the sample to be tested diffracts the X-rays to form diffraction signals; exciting the sample to be detected by the X-rays to form a fluorescent signal;
the computer is connected with an XRF detection subsystem and an XRD detection subsystem of the X-ray diffraction and X-ray fluorescence spectrum synchronous combination system, the XRF detection subsystem is used for obtaining a fluorescence spectrum according to the fluorescence signal, and the XRD detection subsystem is used for obtaining an X-ray diffraction result according to the diffraction signal; the computer is used for obtaining material composition data according to the fluorescence spectrum and the X-ray diffraction result.
According to the specific embodiment provided by the utility model, the utility model discloses the following technical effects:
the utility model relates to an X-ray diffraction and X-ray fluorescence spectrum synchronous combination system; emitting X-rays to the sample to be tested through an X-ray light source subsystem; the sample to be tested diffracts the X-rays to form diffraction signals; exciting the sample to be detected by the X-rays to form a fluorescent signal; obtaining a fluorescence spectrum according to the fluorescence signal through an XRF detection subsystem; obtaining an X-ray diffraction result according to the diffraction signal through an XRD detection subsystem; the utility model realizes the synchronous test of XRD diffraction and XRF fluorescence spectrum at the same position of the sample to be tested.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions of the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present utility model, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a system for simultaneous use of X-ray diffraction and X-ray fluorescence spectroscopy according to the present utility model;
FIG. 2 is a schematic structural diagram of the synchronous combination device of X-ray diffraction and X-ray fluorescence spectrum of the utility model;
FIG. 3 is a schematic diagram of an embodiment of the system for simultaneous X-ray diffraction and X-ray fluorescence spectroscopy of the present utility model.
Symbol description:
the system comprises a sample to be tested-1, a sample stage-2, an X-ray light source subsystem-3, an X-ray light source emitter-31, an X-ray light source bracket-32, an XRF detection subsystem-4, an XRF detector-41, an XRF detector bracket-42, an XRD detection subsystem-5, an XRD detector-51, an XRF detector bracket-52, a safety shell-6 and a computer-7.
Detailed Description
The following description of the embodiments of the present utility model 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 utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
The utility model aims to provide an X-ray diffraction and X-ray fluorescence spectrum synchronous combination system and device, which realize synchronous testing of XRD diffraction and XRF fluorescence spectrum at the same position of a sample to be tested.
In order that the above-recited objects, features and advantages of the present utility model will become more readily apparent, a more particular description of the utility model will be rendered by reference to the appended drawings and appended detailed description.
As shown in FIG. 1, the X-ray diffraction and X-ray fluorescence spectrum synchronous combination system of the utility model; the sample 1 to be measured is placed on a sample table 2; the X-ray diffraction and X-ray fluorescence spectrum synchronous combination system comprises an X-ray light source subsystem 3, an XRF detection subsystem 4 and an XRD detection subsystem 5.
The X-ray light source subsystem 3 is used for emitting X-rays to the sample 1 to be tested; the sample 1 to be tested diffracts the X-rays to form diffraction signals; the X-rays excite the sample 1 to be tested to form fluorescent signals.
The XRF detection subsystem 4 is disposed on the sample stage 2; the XRF detection subsystem 4 is used for obtaining a fluorescence spectrum according to the fluorescence signal; the sample stage 2 is arranged on the transmission optical path of the X-rays.
The XRD detection subsystem 5 is arranged on a transmission light path of the diffraction signal; the XRD detection subsystem 5 is used for obtaining an X-ray diffraction result according to the diffraction signal.
The sample 1 to be measured may be powder, block, fiber, film, liquid or colloid, etc., and is not limited to the above-mentioned types, and may be adjusted according to actual needs.
Preferably, the X-ray source subsystem 3 comprises an X-ray source emitter 31 and an X-ray source holder 32.
The X-ray source emitter 31 is for emitting X-rays toward the sample 1 to be measured.
The X-ray source holder 32 is used for fixing the X-ray source emitter 31.
In the specific embodiment, the X-ray source emitter 31 uses a molybdenum target. Meanwhile, the X-ray source emitter 31 covers 20 °; the X-ray source emitter 31 is placed at a distance of 50mm from the centre of the sample stage 2. In addition, the X-ray source holder 32 is formed by 3D printing. The X-ray source holder 32 is fixed to the bottom plate of the safety housing 6 by screws.
To enable energy dispersive X-ray fluorescence spectroscopy testing, the XRF detection subsystem 4 includes an XRF detector 41 and an XRF detector holder 42.
The XRF detector 41 is used to obtain a fluorescence spectrum from the fluorescence signal.
The XRF detector support 42 is arranged on the sample stage 2; the XRF detector holder 42 is used for holding the XRF detector 41.
For the specific embodiment, the XRF detector 41 is an SDD detector. Meanwhile, the XRF detector 41 is fixed on an XRF detector bracket 42; the XRF detector 41 is located 30mm directly above the centre of the sample stage 2. The XRF detector support 42 is 3D printed. The XRF detector support 42 is fixed to the sample stage 2. The sample stage 2 is fixed on an electric lifting table on the bottom plate of the safety housing 6.
In addition, the XRF detector 41 has an energy resolving function.
Optionally, the XRF detector 41 is a Si-PIN detector or an SDD detector.
To achieve X-ray diffraction testing in the photographic mode, the XRD detection subsystem 5 includes an XRD detector 51 and an XRD detector support 52.
The XRD detector 51 is arranged on a transmission light path of the diffraction signal, and the XRD detector 51 is used for obtaining an X-ray diffraction result according to the diffraction signal.
The XRD detector support 52 is used to hold the XRD detector 51.
By way of example of a specific embodiment, the XRD detector 51 employs a MythenID detector. The MythenID probe consists of 640 sub-probes of size 4mm x 0.05 mm. The XRD detector 51 is mounted on an XRD detector support 52. The XRD detector 51 is located at a distance of 90.7mm from the centre point of the sample stage 2. At the same time, the XRD detector 51 covers a range of 20 (15 to 35). In addition, the XRD detector support 52 is 3D printed. The XRD detector support 52 is screwed onto the floor of the safety housing 6.
Optionally, the XRD detector 51 is a one-dimensional array detector or a two-dimensional array detector.
Meanwhile, the materials of construction of the X-ray source holder 32, the XRF detector holder 42, and the XRD detector holder 52 are metal or plastic; can be adjusted according to specific requirements and is not limited to the two materials.
To prevent the hidden trouble of radiation, the system for synchronously combining the X-ray diffraction and the X-ray fluorescence spectrum also comprises a safety shell 6. The safety housing 6 is internally provided with the X-ray light source subsystem 3, the XRF detection subsystem 4 and the XRD detection subsystem 5.
The safety shell 6 is a customized lead-containing steel plate shell and is used for preventing X-rays from leaking out in the test process.
Taking a specific embodiment as an example, as shown in fig. 3:
the X-ray source emitter 31 adopts a molybdenum target, takes coverage of 20 degrees as an example, is fixed on the X-ray source bracket 32 and is placed at the position of 50mm away from the center of the sample stage 2; the X-ray light source bracket 32 is formed by 3D printing and is fixed on the bottom plate of the safety shell 6 through screws; the XRF detector 41 is an SDD detector and is fixed on the XRF detector bracket 42 and is positioned at a distance of 30mm right above the center of the sample table 2; the XRF detector support 42 is formed by 3D printing and is fixed on the sample table 2, and the sample table 2 is fixed on an electric lifting table on the bottom plate of the safety shell 6; the XRD detector 51 adopts a MythenID detector which consists of 640 sub-detectors with the size of 4mm multiplied by 0.05mm, and is fixed on an XRD detector bracket 52 and positioned at the position with the distance of 90.7mm from the center point of the sample stage 2, and covers the range of 20 degrees (15 degrees to 35 degrees); the XRD detector support 52 is 3D printed and screwed onto the floor of the safety housing 6.
The X-ray source emitter 31 is controlled by the computer 7 or manually to emit X-rays; the sample 1 to be tested diffracts X rays to form diffraction signals; exciting a sample 1 to be detected by X rays to form a fluorescent signal; the XRF detector 41 obtains a fluorescence spectrum from the fluorescence signal; the XRD detector 51 obtains an X-ray diffraction result according to the diffraction signal; the computer 7 obtains material composition data from the fluorescence spectrum and the X-ray diffraction result.
Furthermore, the utility model also provides an X-ray diffraction and X-ray fluorescence spectrum synchronous combined device (shown in figure 2), which comprises the X-ray diffraction and X-ray fluorescence spectrum synchronous combined system, a sample table 2 and a computer 7.
The sample table 2 is used for placing a sample 1 to be tested; the XRF detection subsystem 4 of the synchronous combination system of X-ray diffraction and X-ray fluorescence spectrum is arranged on the sample table; the X-ray light source subsystem 3 of the synchronous combination system of X-ray diffraction and X-ray fluorescence spectrum is used for emitting X-rays to the sample 1 to be detected on the sample table; the sample 1 to be tested diffracts the X-rays to form diffraction signals; the X-rays excite the sample 1 to be tested to form fluorescent signals.
The computer 7 is connected with an XRF detection subsystem 41 and an XRD detection subsystem 51 of the X-ray diffraction and X-ray fluorescence spectrum synchronous combination system, the XRF detection subsystem 41 is used for obtaining a fluorescence spectrum according to the fluorescence signal, and the XRD detection subsystem 51 is used for obtaining an X-ray diffraction result according to the diffraction signal; the computer 7 is used for obtaining material composition data according to the fluorescence spectrum and the X-ray diffraction result.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the system disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the system part.
The specific examples are presented herein to illustrate the principles and embodiments of the present utility model; also, it is within the scope of the present utility model to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the utility model.
Claims (5)
1. An X-ray diffraction and X-ray fluorescence spectrum synchronous combination system is characterized in that a sample to be detected is placed on a sample table; the X-ray diffraction and X-ray fluorescence spectrum synchronous combination system comprises:
an X-ray light source subsystem for emitting X-rays to the sample to be measured; the sample to be tested diffracts the X-rays to form diffraction signals; exciting the sample to be detected by the X-rays to form a fluorescent signal; the X-ray source subsystem comprises: an X-ray light source emitter for emitting X-rays to the sample to be measured; an X-ray light source bracket for fixing the X-ray light source emitter; the X-ray light source emitter is arranged at the position which is 50mm away from the center of the sample table;
the XRF detection subsystem is arranged on the sample platform and is used for obtaining a fluorescence spectrum according to the fluorescence signal; the sample stage is arranged on a transmission light path of the X-rays; the XRF detection subsystem includes: an XRF detector for obtaining a fluorescence spectrum from the fluorescence signal; an XRF detector holder, disposed on the sample stage, for holding the XRF detector; the XRF detector is fixed on the XRF detector support; the XRF detector is positioned at a position which is 30mm away from the center of the sample platform;
the XRD detection subsystem is arranged on a transmission light path of the diffraction signal and is used for obtaining an X-ray diffraction result according to the diffraction signal; the XRD detection subsystem comprises: the XRD detector is arranged on a transmission light path of the diffraction signal and is used for obtaining an X-ray diffraction result according to the diffraction signal; the XRD detector bracket is used for fixing the XRD detector; the XRD detector is located at the center point of the sample stage at a distance of 90.7 mm.
2. The X-ray diffraction and X-ray fluorescence spectroscopy simultaneous combination system of claim 1, wherein the XRF detector is a Si-PIN detector or an SDD detector.
3. The synchronous combination system of X-ray diffraction and X-ray fluorescence spectroscopy of claim 1, wherein the XRD detector is a one-dimensional array detector or a two-dimensional array detector.
4. The X-ray diffraction and X-ray fluorescence spectrum simultaneous use system according to claim 1, further comprising:
and the safety shell is internally provided with the X-ray light source subsystem, the XRF detection subsystem and the XRD detection subsystem.
5. The device for synchronously combining the X-ray diffraction and the X-ray fluorescence spectrum is characterized by comprising the following components:
the X-ray diffraction and X-ray fluorescence spectroscopy simultaneous combination system of any one of claims 1-4;
the sample stage is used for placing a sample to be tested; the XRF detection subsystem of the synchronous combination system of X-ray diffraction and X-ray fluorescence spectrum is arranged on the sample table; the X-ray light source subsystem of the X-ray diffraction and X-ray fluorescence spectrum synchronous combination system is used for emitting X-rays to the sample to be detected on the sample table; the sample to be tested diffracts the X-rays to form diffraction signals; exciting the sample to be detected by the X-rays to form a fluorescent signal;
the computer is connected with an XRF detection subsystem and an XRD detection subsystem of the X-ray diffraction and X-ray fluorescence spectrum synchronous combination system, the XRF detection subsystem is used for obtaining a fluorescence spectrum according to the fluorescence signal, and the XRD detection subsystem is used for obtaining an X-ray diffraction result according to the diffraction signal; the computer is used for obtaining material composition data according to the fluorescence spectrum and the X-ray diffraction result.
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