CN114878609A - X-ray diffraction testing device and method - Google Patents
X-ray diffraction testing device and method Download PDFInfo
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- CN114878609A CN114878609A CN202210492623.XA CN202210492623A CN114878609A CN 114878609 A CN114878609 A CN 114878609A CN 202210492623 A CN202210492623 A CN 202210492623A CN 114878609 A CN114878609 A CN 114878609A
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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
- G01N23/2055—Analysing diffraction patterns
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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
- G01N23/20025—Sample holders or supports therefor
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Abstract
The invention relates to an X-ray diffraction testing device and method, belonging to the technical field of X-ray diffraction, and comprising an X-ray source, a sample stage, a one-dimensional X-ray detector, an angle gauge and a computer, wherein the X-ray source, the sample stage and the one-dimensional X-ray detector all rotate around the axis of the angle gauge, and the one-dimensional X-ray detector is used for acquiring diffraction signals at each rotation angle by adopting a photographic method. Because the one-dimensional X-ray detector adopts a photographic method to collect diffraction signals within a certain angle range at one time, the one-dimensional X-ray detector does not need to carry out pre-scanning and end-scanning in a scanning mode, and the moving times are few, so the testing speed is very high and can reach the second level.
Description
Technical Field
The invention relates to the technical field of X-ray diffraction, in particular to an X-ray diffraction testing device and method.
Background
The X-ray diffractometer accurately measures the crystal structure, texture and stress of a substance by utilizing the diffraction principle, thereby accurately performing phase analysis. The method is used as a main means for representing the crystal structure of the material, and is widely applied to aspects of scientific research, inspection and detection, quality control of enterprises on products and the like.
The current mainstream test method of the X-ray diffractometer is a diffractometer method, namely, a point detector is driven by an angle meter to stay for a certain time at different angles, then diffraction signals are scanned and collected, and then an angle-intensity curve is processed by a computer. The starting and stopping steps required by the testing method enable the testing speed of the X-ray diffractometer to be slow, and the testing requirements cannot be well met.
Therefore, an apparatus and a method for testing X-ray diffraction with fast detection speed and satisfying the testing requirement are needed.
Disclosure of Invention
The invention aims to provide an X-ray diffraction testing device and method, which are used for improving the speed of measuring substances by X-ray diffraction and meeting the testing requirement.
In order to achieve the purpose, the invention provides the following scheme:
an X-ray diffraction test apparatus comprising:
an angle gauge;
an X-ray source is arranged outside the frame of the goniometer;
a sample table is arranged on the inner side of the frame of the goniometer;
a one-dimensional X-ray detector is arranged on the outer side of the frame of the sample stage;
the X-ray source, the sample stage and the one-dimensional X-ray detector all rotate around the axis of the goniometer;
the X-ray source is used for irradiating a sample to be detected placed on the sample stage so as to enable the sample to be detected to generate a diffraction signal;
the one-dimensional X-ray detector is used for acquiring the diffraction signal under each rotation angle by adopting a photographic method to obtain each first diffraction pattern;
the one-dimensional X-ray detector is connected with a computer;
the computer is used for generating an X-ray diffraction graph according to each rotation angle and each first diffraction pattern.
An X-ray diffraction test method using the X-ray diffraction test apparatus, comprising:
irradiating a sample to be detected placed on a sample table by an X-ray source to enable the sample to be detected to generate a diffraction signal;
the one-dimensional X-ray detector acquires the diffraction signal under each rotation angle by adopting a photographic method to obtain each first diffraction pattern;
and generating an X-ray diffraction graph by the computer according to each rotation angle and each first diffraction graph.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention provides an X-ray diffraction testing device and method, because the one-dimensional X-ray detector adopts a photographic method to collect diffraction signals within a certain angle range at one time, because pre-scanning and ending scanning in a scanning mode are not needed, and the moving times are few, the testing speed is very high, and can reach the second level.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts. The following drawings are not necessarily to scale, emphasis instead being placed upon illustrating the principles of the invention.
Fig. 1 shows a schematic view of an X-ray diffraction test apparatus provided in accordance with embodiment 1 of the present invention;
fig. 2 shows a flowchart of an X-ray diffraction test method provided in embodiment 2 of the present invention.
Description of the symbols:
1-a light source arm; 2-a sample stage; 3-a detector arm; 4-goniometer; 5-an X-ray source; 6-one-dimensional X-ray detector.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
As used in this disclosure and in the claims, the terms "a," "an," "the," and/or "the" are not intended to be inclusive in the singular, but rather are inclusive in the plural, unless the context clearly dictates otherwise. In general, the terms "comprises" and "comprising" merely indicate that steps and elements are included which are explicitly identified, that the steps and elements do not form an exclusive list, and that a method or apparatus may include other steps or elements.
Although the present invention makes various references to certain modules in a system according to embodiments of the present invention, any number of different modules may be used and run on a user terminal and/or server. The modules are merely illustrative and different aspects of the systems and methods may use different modules.
Flow charts are used in the present invention to illustrate the operations performed by an apparatus according to embodiments of the present invention. It should be understood that the preceding or following operations are not necessarily performed in the exact order in which they are performed. Rather, the various steps may be processed in reverse order or simultaneously, as desired. Meanwhile, other operations may be added to the processes, or a certain step or several steps of operations may be removed from the processes.
The invention aims to provide an X-ray diffraction testing device and method to improve the speed of measuring substances by X-ray diffraction and meet the testing requirement
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1:
the earliest X-ray diffraction test methods were photographic methods, i.e., negative exposure was used to collect the diffraction signals emitted by the sample after X-ray irradiation, followed by phase-washing and further drawing the angle-intensity curves with a ruler. In order to increase the detection angle range, the debye-scherrer method using a curved plate has been developed in addition to the earliest planar plate method, and is more suitable for powder sample testing. However, the photographic process is cumbersome and has low precision, and thus has been rarely used.
And most tests need a certain range of qualitative or semi-quantitative tests, and do not need a large angle range and angle resolution, for example, in the process of drug production, scanning is only needed within the range of 10-40 degrees and the step length of 0.05-0.08 degree, and whether the crystal form of the product meets the requirements can be known by observing whether three or five main diffraction peaks appear.
With the increasing application of X-ray diffraction, the testing requirement of X-ray diffraction is increased, and the testing speed of a diffractometer is also required to be increased. On the one hand, diffractometer manufacturers have developed X-ray sources 5 with greater power, and on the other hand, have introduced one-dimensional X-ray detectors 6. The one-dimensional detector adopts a scanning mode during testing, namely each sub-detector stays for a certain time at different angles in a testing range to collect diffraction signals, and finally a computer superposes and processes the signals of all the sub-detectors to form an angle-intensity curve. Because the plurality of sub-detectors work together, even if the residence time of each sub-detector is short, the residence time after superposition is equivalent to long, so the test efficiency is greatly improved, and the test time of the point detector from dozens of minutes to dozens of minutes can be shortened to several to dozens of minutes.
With the increasing sample amount of X-ray diffraction in scientific research and production, the testing speed of the existing diffractometer based on the scanning mode of the one-dimensional detector can reach several minutes, but the testing requirement can not be well met.
The current common method for commercializing the one-dimensional detector of the diffractometer is to scan it at a remote location and require start and stop steps so that its test speed cannot be too fast.
In order to increase the testing speed and achieve the requirement of qualitative or semi-quantitative testing range, referring to fig. 1, the present embodiment provides an X-ray diffraction testing apparatus, including:
an goniometer 4;
a light source arm 1 is arranged outside the frame of the goniometer 4;
an X-ray source 5 is arranged on the light source arm 1;
a sample table 2 is arranged on the inner side of the frame of the goniometer 4;
a detector arm 3 is arranged outside the frame of the sample table 2; a one-dimensional X-ray detector 6 is arranged on the detector arm 3, and the distance between the one-dimensional X-ray detector 6 and the sample table 2 is preferably 50-300 mm; (ii) a
The light source arm 1, the sample table 2 and the detector arm 3 all rotate around the axis of the goniometer 4; the sample stage 2 is located at the middle position between the X-ray source 5 and the one-dimensional X-ray detector 6;
the X-ray source 5 is used for irradiating a sample to be detected placed on the sample stage 2 so as to enable the sample to be detected to generate a diffraction signal;
the one-dimensional X-ray detector 6 is used for acquiring the diffraction signal at each rotation angle by adopting a photographic method to obtain each first diffraction pattern;
the one-dimensional X-ray detector 6 is connected with a computer;
the computer is used for generating an X-ray diffraction graph according to each rotation angle and each first diffraction pattern.
It should be noted that the X-ray diffraction testing apparatus of the present embodiment further includes other structures and accessories that are necessary for the X-ray diffractometer but are not critical in the present embodiment, and are not described herein;
as an alternative embodiment, the one-dimensional X-ray detector 6 comprises a plurality of sub-detectors.
As an optional implementation manner, the difference between the angle of each sub-detector and the position of the sample to be measured remains two decimal places, and the difference between the angle of each sub-detector and the angle of the adjacent sub-detector also remains two decimal places.
The photographic method mentioned in the present example is distinguished from the scanning method in that: the photography method is to receive diffraction information once, and the scanning method is to superpose the multi-point scanning results to obtain the diffraction information. In addition, the conventional Debye photography method usually uses a ring-shaped negative film, so the sub-detectors of the multi-step approximate Debye photography in this embodiment should also be arranged in an arc shape. However, the existing one-dimensional X-ray detector 6 has high enough precision, enough sub-detectors, and small enough width of a single sub-detector, and the arc length is approximately equal to the chord length when the distance between two points on the arc is close enough, so the sub-detectors of the one-dimensional X-ray detector 6 in this embodiment are arranged in an arc or linear manner.
In the embodiment, the distance between the X-ray source 5 and the sample stage 2 is preferably set to be 50-300mm, so that the one-time coverage angle of the detector is larger than that of the traditional scanning mode, and the actual angle corresponding to each sub-detector can be approximately linearly distributed.
Similar to the conventional X-ray debye photography, the positions of the X-ray source 5, the sample stage 2 and the one-dimensional X-ray detector 6 are fixed during each rotation angle test, and the detector arm 3 moves to the next rotation angle after each rotation angle test, so that the angle ranges of the detectors of the one-dimensional X-ray detector 6 are different.
In order to make the X-ray diffraction test apparatus of the present application more clear to those skilled in the art, the following description will be given by way of specific examples.
DX2700 diffractometer manufactured by Dandonghaoyuan instruments, Inc. is taken as an example. The instrument is provided with a 3KW X-ray source 5 and a Mythen1D detector, wherein the latter comprises 640 sub-detectors with the width of 0.05mm, when the one-dimensional detector is placed at a position 286.5mm away from a sample through modification, the actual angle difference between the position of each sub-detector and the position of the sample is taken to be the second position after the decimal point, and the angle difference between every two adjacent sub-detectors is also taken to be the second position after the decimal point, so that the consistency of the angle difference calculated by adopting the interval of 0.01 degrees is ensured.
For example, the following steps are carried out: the actual corresponding angle difference between the sub-detector 160 pixels away from the center of the one-dimensional detector and the central pixel is 1.599 degrees, and the second position is 1.60 degrees after the sub-detector is approximated to a decimal point. The sub-detector with 320 pixels from the center of the one-dimensional detector, namely the edge-most sub-detector, has an actual corresponding angle difference of 3.1964 degrees with the center pixel, and the second position is 3.20 degrees after the approximation to a decimal point. Because, the one-dimensional detector can obtain better diffraction signals within the range of 6.4 degrees at most once.
In order to expand the test range, a multistep approximately Debye photographic method is adopted, namely, the method is realized by taking pictures at a plurality of positions so as to solve the problem of small angle range of single-time taking.
For example, the following steps are carried out: after a sample is placed, the detector is respectively moved to 13.2 degrees, 19.6 degrees, 26.0 degrees, 32.4 degrees and 38.8 degrees, a diffraction pattern is respectively shot in ten seconds, and then a large-range diffraction pattern within the range of 10 degrees to 42 degrees can be spliced; meanwhile, the angle difference corresponding to each data point is 0.01 degrees, so that the resolution is higher. The entire test time takes less than one minute (fifty seconds, with about 1 second of detector travel time between each angle), much faster than current one-dimensional detector scan patterns.
In this embodiment, since the plurality of sub-detectors are linearly arranged to form a certain length, the one-dimensional X-ray detector 6 moves the sub-detectors by the total length of each step, the rotation angle is large, the number of times of movement is small, diffraction data results do not need to be superimposed, and an angle/diffraction intensity map can be obtained only by splicing. And the photographic method is adopted, pre-scanning and ending scanning in a scanning mode are not needed, and the moving times are few, so that the testing speed is very high and can reach the second level. And meanwhile, included angles between each sub-detector and diffraction signals are designed in advance according to the peak output range of the sample to be tested, so that qualitative or quantitative testing can be realized.
Example 2:
in the conventional scanning method, the detector rotates to receive signals in a small step (small rotation angle), the X-ray source 5 needs to be started and stopped each time the detector rotates, and finally, data of the sub-detectors are superposed to obtain an angle/diffraction intensity graph. The method needs starting and stopping steps, so that the testing speed is slow, and the testing requirement cannot be well met. In this regard, the present embodiment provides an X-ray diffraction test method using the test apparatus provided in embodiment 1, as shown in fig. 2, including:
s1: the X-ray source 5 irradiates a sample to be detected placed on the sample stage 2, so that the sample to be detected generates a diffraction signal;
s2: the one-dimensional X-ray detector 6 acquires the diffraction signal under each rotation angle by adopting a photographic method to obtain each first diffraction pattern;
s3: the computer generates an X-ray diffraction curve graph according to each rotation angle and each first diffraction pattern;
since the one-dimensional X-ray detector 6 of the present embodiment includes a plurality of sub-detectors arranged in an arc or linear manner, the S2 and S3 specifically further include: calculating the included angle between each sub-detector and the diffraction signal in advance according to the position of the one-dimensional X-ray detector 6 so as to cover all peak-appearing ranges of the sample; and finally, splicing the angle/intensity X-ray diffraction curve subgraphs to obtain a high-resolution X-ray diffraction curve graph in a large angle range.
The test method of the embodiment changes the scanning method into the photographic method, and has high test speed; meanwhile, the problems of small angle range and low angle resolution existing in a single photographing method are solved through a multi-step photographing mode. The method is suitable for the condition that the requirement on the test precision is not good, but the test speed is required to be fast.
The present invention has been described using specific terms to describe embodiments of the invention. Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The foregoing is illustrative of the present invention and is not to be construed as limiting thereof. Although a few exemplary embodiments of this invention have been described, those skilled in the art will readily appreciate that many modifications are possible in the exemplary embodiments without materially departing from the novel teachings and advantages of this invention. Accordingly, all such modifications are intended to be included within the scope of this invention as defined in the claims. It is to be understood that the foregoing is illustrative of the present invention and is not to be construed as limited to the specific embodiments disclosed, and that modifications to the disclosed embodiments, as well as other embodiments, are intended to be included within the scope of the appended claims. The invention is defined by the claims and their equivalents.
Claims (8)
1. An X-ray diffraction test apparatus, comprising:
an angle gauge;
an X-ray source is arranged outside the frame of the goniometer;
a sample table is arranged on the inner side of the frame of the goniometer;
a one-dimensional X-ray detector is arranged on the outer side of the frame of the sample stage;
the X-ray source, the sample stage and the one-dimensional X-ray detector all rotate around the axis of the goniometer;
the X-ray source is used for irradiating a sample to be detected placed on the sample stage so as to enable the sample to be detected to generate a diffraction signal;
the one-dimensional X-ray detector is used for acquiring the diffraction signal under each rotation angle by adopting a photographic method to obtain each first diffraction pattern;
the one-dimensional X-ray detector is connected with a computer;
the computer is used for generating an X-ray diffraction graph according to each rotation angle and each first diffraction pattern.
2. The X-ray diffraction test apparatus of claim 1, wherein the one-dimensional X-ray detector comprises a plurality of sub-detectors; the sub-detectors are arranged in an arc or linear manner.
3. The X-ray diffraction testing device of claim 1, wherein a light source arm is disposed outside the frame of the goniometer; the light source arm is used for placing the X-ray source.
4. The X-ray diffraction testing apparatus of claim 1, wherein a detector arm is disposed outside the frame of the sample stage; the detector arm is used for placing the one-dimensional X-ray detector.
5. The X-ray diffraction testing device of claim 2, wherein the angular difference between the position of each sub-detector and the position of the sample to be tested remains two decimals.
6. The X-ray diffraction test device of claim 2, wherein the angular difference between the position of each sub-detector and the position of the adjacent sub-detector remains two decimals.
7. An X-ray diffraction test method using the X-ray diffraction test apparatus according to any one of claims 1 to 6, comprising:
irradiating a sample to be detected placed on a sample table by an X-ray source to enable the sample to be detected to generate a diffraction signal;
the one-dimensional X-ray detector acquires the diffraction signal under each rotation angle by adopting a photographic method to obtain each first diffraction pattern;
and generating an X-ray diffraction graph by the computer according to each rotation angle and each first diffraction graph.
8. The X-ray diffraction test method of claim 7, wherein the photographic method is a multi-step approximation debye photographic method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210492623.XA CN114878609A (en) | 2022-05-07 | 2022-05-07 | X-ray diffraction testing device and method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210492623.XA CN114878609A (en) | 2022-05-07 | 2022-05-07 | X-ray diffraction testing device and method |
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Application publication date: 20220809 |