CN110596162A - Calibration device based on monochromatic X-ray diffraction - Google Patents
Calibration device based on monochromatic X-ray diffraction Download PDFInfo
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- CN110596162A CN110596162A CN201910884267.4A CN201910884267A CN110596162A CN 110596162 A CN110596162 A CN 110596162A CN 201910884267 A CN201910884267 A CN 201910884267A CN 110596162 A CN110596162 A CN 110596162A
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- polycrystalline powder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
Abstract
The invention discloses a single crystal/oriented crystal calibration device based on monochromatic X-ray diffraction, wherein a base material comprises an upper surface and a lower surface; the adhesive layer is configured to fix the calibration device on the surface of the sample subjected to X-ray diffraction, and the adhesive layer is arranged on the lower surface; a layer of polycrystalline powder is provided on the upper surface, the layer of polycrystalline powder having a thickness less than one fifth of the depth of penetration of the polycrystalline powder by X-rays such that a first diffraction signal from the surface of the sample and a second diffraction signal from the polycrystalline powder are acquired simultaneously.
Description
Technical Field
The invention belongs to the technical field of diffraction measurement, and particularly relates to a calibration device based on monochromatic X-ray diffraction.
Background
The X-ray diffractometer uses an X-ray light source to perform diffraction experiments, collects rays generated in the experiments, and collects the rays as diffraction spectrums. By analyzing the diffraction spectrum, phase identification and stress analysis can be performed on the sample. If the diffractometer is the Laue method, orientation analysis can also be performed. Therefore, the X-ray diffractometer and the analysis technique thereof have wide application in scientific research and industrial production in the fields of metallurgy, materials science, biology and the like.
However, to achieve sufficient analytical accuracy, the X-ray diffractometer needs to be calibrated from time to time, and a common calibration method is to use a standard sample. However, the preparation of the standard sample usually requires a long time, the height of the standard sample is often far different from that of the actually measured sample, and the height of the sample still needs to be further adjusted after calibration, which affects the precision of the sample. Therefore, in order to obtain more accurate precision, the sample to be detected and the standard sample signal are often required to be simultaneously recorded, but the sample to be detected may have a more complex surface appearance, which greatly affects the simultaneous recording. Based on the practical problem, a diffractometer calibration device needs to be developed, can conveniently calibrate under various diffraction geometries, and has the characteristics of convenience in use and time saving.
The above information disclosed in this background section is only for enhancement of understanding of the background of the invention and therefore it may contain information that does not form the prior art that is already known in this country to a person of ordinary skill in the art.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the calibration device based on the monochromatic X-ray diffraction, which simplifies the measurement requirement, can conveniently calibrate under various diffraction geometries, and has the characteristics of convenient use and time saving.
The invention aims to realize the technical scheme that the calibration device based on the monochromatic X-ray diffraction comprises,
a substrate comprising an upper surface and a lower surface;
an adhesive layer configured to fix the calibration device to the surface of the sample for X-ray diffraction, the adhesive layer being provided on the lower surface;
a polycrystalline powder layer disposed on the upper surface, the polycrystalline powder layer having a thickness less than one fifth a depth of penetration of the polycrystalline powder by X-rays such that a first diffraction signal from the sample surface and a second diffraction signal from the polycrystalline powder are simultaneously acquired.
In the calibration arrangement, the calibration arrangement comprises an attachment layer for attaching the polycrystalline powder layer to the upper surface, the thickness of the polycrystalline powder layer being less than one tenth of the penetration depth of X-rays through the polycrystalline powder layer such that a first diffraction signal from the sample surface and a second diffraction signal from the sample surface are acquired simultaneously.
In the calibration device, the thickness of the polycrystalline powder layer is one fifth to one tenth of the penetration depth of X-rays to the polycrystalline powder.
In the calibration device, the polycrystalline powder layer comprises a discontinuous area which is arranged in the polycrystalline powder layer and is completely transparent to X-rays, so that when an incident beam of the X-rays moves to the discontinuous area, a second diffraction signal stops being collected.
In the calibration device, the polycrystalline powder comprises alumina powder, silicon powder, calcium carbonate powder and/or lithium lanthanum zirconium oxide powder.
In the calibration device, the polycrystalline powder layer comprises a thickened area with the thickness larger than one fifth of the penetration depth of X-rays on the polycrystalline powder, so that the first diffraction signal from the surface of the sample stops being acquired.
In the calibration device, the base material is made of transparent material.
In the calibration device, the calibration device is an adhesive tape.
In the calibration device, the polycrystalline powder layer is formed by spraying a solution, an emulsion or a suspension of polycrystalline powder on the upper surface and then drying.
In the calibration device, the adhesive layer is provided with scales.
Compared with the prior art, the invention has the following advantages:
according to the invention, the polycrystalline powder for calibration is placed in the adhesive tape which can be freely adhered to the surface to be calibrated in advance, so that the advantages of convenience in use, use time saving and convenience in fixation for complex surfaces and non-horizontal surfaces can be achieved.
Drawings
Various other advantages and benefits of the present invention will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. It is obvious that the drawings described below are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. Also, like parts are designated by like reference numerals throughout the drawings.
In the drawings:
FIG. 1 is a schematic structural diagram of a calibration apparatus for performing monochromatic X-ray diffraction-based calibration according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a calibration apparatus for performing monochromatic X-ray diffraction-based calibration according to an embodiment of the present invention.
The invention is further explained below with reference to the figures and examples.
Detailed Description
Specific embodiments of the present invention will be described in more detail below with reference to fig. 1 to 2. While specific embodiments of the invention are shown in the drawings, it should be understood that the invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
It should be noted that certain terms are used throughout the description and claims to refer to particular components. As one skilled in the art will appreciate, various names may be used to refer to a component. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. The description which follows is a preferred embodiment of the invention, but is made for the purpose of illustrating the general principles of the invention and not for the purpose of limiting the scope of the invention. The scope of the present invention is defined by the appended claims.
For the purpose of facilitating understanding of the embodiments of the present invention, the following description will be made by taking specific embodiments as examples with reference to the accompanying drawings, and the drawings are not to be construed as limiting the embodiments of the present invention.
For better understanding, as shown in fig. 1, a calibration device based on monochromatic X-ray diffraction comprises a substrate 1, which comprises an upper surface and a lower surface;
an adhesive layer 4 configured to fix the calibration device to the surface of the sample for X-ray diffraction, the adhesive layer 4 being provided on the lower surface;
a polycrystalline powder layer 3 provided on the upper surface, the polycrystalline powder layer 3 having a thickness of less than one fifth of a penetration depth of the polycrystalline powder by the X-rays such that a first diffraction signal from the sample surface and a second diffraction signal from the polycrystalline powder are simultaneously acquired.
To further understand the present invention, in one embodiment, a diffractometer calibration tape is provided, which includes a substrate 1, an adhesion layer 2 for adhering polycrystalline powder, a polycrystalline powder layer 3, and an adhesion layer 4 such as an adhesive layer for adhering to a calibration surface. When in use, the adhesive tape is adhered to the surface to be calibrated, and the calibration can be completed by using the calibration method of the X-ray diffractometer.
In a preferred embodiment, the polycrystalline powder layer 3 is made of alumina powder or silicon powder.
In a preferred embodiment, the polycrystalline powder layer 3 has discrete regions 5 of a discontinuous layer as shown in FIG. 2. The discontinuous layer is capable of transmitting X-rays completely, such that the polycrystalline powder layer signals are not received when the incident beam moves to the location of the discontinuous layer.
In a preferred embodiment, the thickness d of the layer 3 of polycrystalline powder should be less than one fifth to one tenth of the penetration depth of the ray into the polycrystalline powder. The signal of the sample to be tested and the signal of the polycrystalline powder can be collected simultaneously, so that the calibration signal can be conveniently collected when the sample is tested, and the method is used for testing with high precision.
A tape for calibrating diffractometers, the thickness d of the layer 3 of polycrystalline powder should be greater than one fifth of the penetration depth of the rays into the polycrystalline powder. Diffraction signals from the polycrystalline powder layer can now be collected with sufficiently high intensity for a more accurate calibration.
According to the invention, the polycrystalline powder for calibration is placed in the adhesive tape which can be freely adhered to the surface to be calibrated in advance, so that the advantages of convenience in use, use time saving and convenience in fixation for complex surfaces and non-horizontal surfaces can be achieved.
In a preferred embodiment of the calibration arrangement, the calibration arrangement comprises an attachment layer 2 for attaching the polycrystalline powder layer 3 to the upper surface, the thickness of the polycrystalline powder layer 3 being smaller than one tenth of the penetration depth of the polycrystalline powder by X-rays such that a first diffraction signal from the sample surface and a second diffraction signal from the sample surface are acquired simultaneously.
In a preferred embodiment of the calibration device, the thickness of the polycrystalline powder layer 3 is one fifth to one tenth of the penetration depth of the polycrystalline powder by the X-rays.
In a preferred embodiment of the calibration arrangement, the polycrystalline powder layer 3 comprises discrete areas 5 arranged therein, which are completely transparent to X-rays, such that the acquisition of the second diffraction signal is stopped when the incident beam of X-rays moves to the discrete areas 5.
In a preferred embodiment of the calibration device, the polycrystalline powder comprises alumina powder, silicon powder, calcium carbonate powder and/or lithium lanthanum zirconium oxide powder.
In a preferred embodiment of the calibration arrangement, the layer 3 of polycrystalline powder comprises a thickened area having a thickness larger than one fifth of the penetration depth of the polycrystalline powder by the X-rays, so that the first diffraction signal from the surface of the sample ceases to be acquired.
In a preferred embodiment of the calibration device, the substrate 1 is made of a transparent material.
In a preferred embodiment of the calibration device, the calibration device is an adhesive tape.
In a preferred embodiment of the calibration device, the polycrystalline powder layer 3 is formed by spraying a solution, an emulsion or a suspension of the polycrystalline powder onto the upper surface and then drying the solution, the emulsion or the suspension.
In a preferred embodiment of the calibration device, the adhesive layer 4 is provided with scales.
Although the embodiments of the present invention have been described above with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments and application fields, and the above-described embodiments are illustrative, instructive, and not restrictive. Those skilled in the art, having the benefit of this disclosure, may effect numerous modifications thereto without departing from the scope of the invention as defined by the appended claims.
Claims (10)
1. A calibration device based on monochromatic X-ray diffraction comprises,
a substrate comprising an upper surface and a lower surface;
an adhesive layer configured to fix the calibration device to the surface of the sample for X-ray diffraction, the adhesive layer being provided on the lower surface;
a polycrystalline powder layer disposed on the upper surface, the polycrystalline powder layer having a thickness less than one fifth a depth of penetration of the polycrystalline powder by X-rays such that a first diffraction signal from the sample surface and a second diffraction signal from the polycrystalline powder are simultaneously acquired.
2. Calibration arrangement according to claim 1, wherein preferably the calibration arrangement comprises an adhesion layer for adhering the polycrystalline powder layer to the upper surface, the thickness of the polycrystalline powder layer being smaller than one tenth of the penetration depth of X-rays through the polycrystalline powder such that a first diffraction signal from the sample surface and a second diffraction signal from the sample surface are acquired simultaneously.
3. Calibration arrangement according to claim 1, wherein the thickness of the layer of polycrystalline powder is one fifth to one tenth of the penetration depth of the polycrystalline powder by X-rays.
4. Calibration arrangement according to claim 1, wherein the polycrystalline powder layer comprises discrete areas provided therein which are completely transparent to X-rays, such that the second diffraction signal ceases to be acquired when the incident beam of X-rays is moved to said discrete areas.
5. The calibration device as claimed in claim 1, wherein the polycrystalline powder comprises alumina powder, silicon powder, calcium carbonate powder and/or lithium lanthanum zirconium oxygen powder.
6. Calibration arrangement according to claim 1, wherein the polycrystalline powder layer comprises a thickened area with a thickness larger than one fifth of the penetration depth of X-rays into the polycrystalline powder, such that the first diffraction signal from the sample surface ceases to be acquired.
7. The calibration device as defined in claim 1, wherein the substrate is made of a transparent material.
8. The calibration device of claim 1, wherein the calibration device is an adhesive tape.
9. The calibration device according to claim 1, wherein the polycrystalline powder layer is formed by spraying a solution, an emulsion or a suspension of the polycrystalline powder on the upper surface and then drying the solution, the emulsion or the suspension.
10. The calibration device of claim 1, wherein the adhesive layer is provided with a scale.
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| CN201910884267.4A CN110596162B (en) | 2019-09-19 | 2019-09-19 | Calibration device based on monochromatic X-ray diffraction |
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