CN108132484B - Adjusting method of adjustable single crystal monochromator - Google Patents
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Abstract
The embodiment of the invention relates to an adjusting method of an adjustable single crystal monochromator, which comprises the following steps: A. carrying out vacuum pumping operation on the vacuum chamber by using a dry vacuum pump; B. adjusting the relative positions of the open X-ray machine, the single crystal and the detector to enable the center of an emergent port of the open X-ray machine, the center of an incident port of the detector and the center of the single crystal to be on the same horizontal plane; C. starting an open X-ray machine, emitting X-rays, and forming first single-energy X-rays after the X-rays are diffracted by a monocrystal; D. the first monoenergetic X-rays are received by the detector; E. the single crystal and the open type X-ray machine are driven to rotate in a gear linkage mode, and the X-rays form second single-energy X-rays after being diffracted by the single crystal; F. the second monoenergetic X-rays are received by the detector; G. and E, changing an included angle between the X-ray and the single crystal, and repeating the step E and the step F to obtain the single-energy X-ray with different energies. The invention has simple operation, high adjusting precision and small error.
Description
Technical Field
The invention relates to the technical field of measurement, in particular to an adjusting method of an adjustable single crystal monochromator.
Background
In the research field of single-energy X-ray, X-ray is diffracted by a single crystal Bragg to form a certain single-energy X-ray, and then the X-ray is captured by a detector. In order to generate bragg diffraction, the bragg condition, which is the coherent superposition of the single crystal on the reflection of X-rays, must be satisfied. Two different ways are usually chosen to consider such coherent superposition, one of which is to fix the facets, X-rays are incident at different angles, and the reflection between different facets is coherent and intensified if the difference in wavelength is exactly an integral multiple; another way is to consider only facets perpendicular to the direction of incidence, and coherence intensifies if such facet spacings are integer multiples of half a wavelength. The coherence enhancement conditions obtained in these two ways are equivalent and are referred to as bragg conditions.
That is, during the study of monoenergetic X-rays, the angle between the single crystal and the incident X-rays needs to be constantly changed. In the prior art, the angle of the crystal is controlled by controlling the front-back distance of the linkage rod by often adopting a linkage mode of the support rod for adjustment. However, the linkage mode of the supporting rods is not only high in processing difficulty of the device, but also cannot be adjusted when errors occur in the adjusting process, so that the influence on optical precision experiments is great. Therefore, there is a need for a method of adjusting a single crystal monochromator that can solve the above-mentioned problems.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides an adjusting method of an adjustable single crystal monochromator, which can control the adjusting precision, reduce the error and enhance the signal intensity received by a detector.
To achieve the above object, the present invention provides an adjusting method of an adjustable single crystal monochromator, the adjusting method comprising:
step A, carrying out vacuum pumping operation on a vacuum chamber by using a dry vacuum pump;
b, adjusting the relative positions of the open X-ray machine, the single crystal and the detector to enable the center of an emergent port of the open X-ray machine, the center of an incident port of the detector and the center of the single crystal to be positioned on the same horizontal plane;
step C, starting the open type X-ray machine, emitting X-rays, forming a first diffraction angle between the X-rays and the single crystal, and forming first monoenergetic X-rays after the X-rays are diffracted by the single crystal;
step D, the first single-energy X-ray is emitted through a beryllium window of the vacuum chamber and received by the detector;
step E, driving the single crystal and the open type X-ray machine to rotate in a gear linkage mode, forming a second diffraction angle between the X-ray and the single crystal, and forming a second mono-energy X-ray after the X-ray is diffracted by the single crystal;
step F, the second single-energy X-ray is emitted through a beryllium window of the vacuum chamber and received by the detector;
and G, changing an included angle between the X-ray and the single crystal, and repeating the step E and the step F to obtain the single-energy X-ray with different energies.
Preferably, the vacuum degree of the vacuum chamber reaches at least 10-5Magnitude.
Preferably, the step C specifically includes:
starting the open X-ray machine to emit the X-ray;
rotating the single crystal in a gear linkage mode, and rotating the open type X-ray machine by a corresponding angle to diffract the X-rays on the single crystal to form a first diffraction angle;
and obtaining a first monoenergetic X-ray after the X-ray is diffracted by the single crystal.
Further preferably, before the step C, the adjusting method further includes:
and adjusting the relative position of the single crystal and the open X-ray machine in a gear linkage mode.
Preferably, the step of rotating the single crystal and the open X-ray machine by using a gear linkage mode respectively specifically comprises:
the driven double gears are driven to rotate through the driving duplicate gear;
the lower gear of the driven double gear drives the single crystal to rotate by a first angle;
and the upper gear of the driven double gear drives the open X-ray machine to rotate by a second angle corresponding to the first angle.
Further preferably, the upper gear and the lower gear of the driven double gear are connected through a rotary support structure.
According to the adjusting method of the adjustable single crystal monochromator provided by the embodiment of the invention, a gear linkage mode is adopted, the driving gear and the driven gear both adopt double gears, two gears of the driven gear are connected by adopting a rotary supporting structure, the upper gear and the lower gear of the driven gear can be ensured to rotate independently, the upper gear drives the optical machine to rotate, the lower gear drives the single crystal to rotate, and the rotating speed ratio between the gears is reasonably designed, so that the included angle between the single crystal and incident X rays can be changed without changing the emergent direction of the X rays. Meanwhile, an open X-ray machine is adopted, so that the vacuum degree can be integrally controlled, and the signal intensity received by the detector is enhanced. The adjusting method is simple to operate and high in adjusting precision, and can control the adjusting precision by changing the rotating speed between the gears, so that errors are reduced.
Drawings
FIG. 1 is a diagram of an X-ray source apparatus employing an adjustment method of an adjustable single crystal monochromator according to an embodiment of the present invention;
fig. 2 is a schematic flow chart of an adjusting method of an adjustable single crystal monochromator according to an embodiment of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
The embodiment of the invention relates to an adjusting method of an adjustable single crystal monochromator, which adopts a gear linkage mode and an open X-ray machine, can realize the change of the included angle between a single crystal and incident X-rays without changing the emergent direction of the X-rays, can integrally control the vacuum degree, and enhances the signal intensity received by a detector.
The adjusting method of the adjustable single crystal monochromator provided by the embodiment of the invention can be applied to an X-ray source device, as shown in figure 1. To facilitate understanding of the method of adjusting the adjustable monochromator according to the invention, a brief description of the X-ray source arrangement to which it is applied follows.
The X-ray source device specifically comprises a base 1, a vacuum chamber 2, a dry vacuum pump 3, an adjustable single crystal monochromator 4, an open X-ray machine 5, a detector 6, a driving motor 7, a magnetic fluid sealing element 8 and a vacuum degree detector 9.
A base 1 of the X-ray source device is provided with a fixed groove 11, and a vacuum chamber 2 is placed in the fixed groove 11. The vacuum chamber 2 includes a cylindrical chamber portion and a hemispherical chamber portion, a connection port 21 and an exit window 22 are formed in the circumferential direction of the cylindrical chamber portion, and a beryllium window (not shown) is provided in the exit window 22. The dry vacuum pump 3 is arranged on the upper surface of the base 1, the dry pump 3 is connected with a connecting port 21 of the vacuum chamber 2, and an incident port of the detector 6 is connected with an exit window 22. An adjustable single crystal monochromator 4 is disposed inside the vacuum chamber 2, and the adjustable single crystal monochromator 4 includes a driving dual gear (not shown), a driven dual gear (not shown), a single crystal 44, and a rotary table 43.
The driving dual gear is meshed with the driven dual gear, the upper gear 42 of the driven dual gear is fixedly connected with the rotating platform 43, the lower gear 41 of the driven dual gear is fixed with a supporting column (not shown in the figure), the supporting column sequentially passes through the upper gear 42 of the driven dual gear and the rotating platform 43 and penetrates out of the rotating platform 43, and the single crystal 44 is fixed on the supporting column. The driving motor 5 is arranged in the base 1, a rotating shaft (not shown in the figure) of the driving motor 5 is connected with the driving duplicate gear for driving the driving duplicate gear to operate, and a magnetic fluid sealing member 8 is arranged between the rotating shaft and the vacuum chamber 2. In addition, a vacuum degree detector 9 can be arranged in the vacuum chamber 2 and used for monitoring the vacuum degree in the vacuum chamber 2 in real time and detecting the tightness problem of the vacuum chamber 2 at regular time.
Fig. 2 is a schematic flow chart of an adjusting method of an adjustable single crystal monochromator according to an embodiment of the present invention. As shown in fig. 2:
and 101, performing vacuum pumping operation on the vacuum chamber by using a dry vacuum pump.
Specifically, the vacuum degree of the vacuum chamber reaches at least 10-5Magnitude.
In a specific process, an open X-ray machine is adopted, namely a beryllium window of the X-ray machine is removed, the open X-ray machine is placed in a vacuum chamber, so that the vacuum interior of the X-ray machine is communicated with the vacuum chamber, the control of the overall vacuum degree is realized, the overall vacuum degree is easy to master, the beryllium window of the X-ray machine is removed, the times of X-rays penetrating through the beryllium window are reduced, and the signal intensity received by a detector is enhanced. Preferably, the vacuum chamber is evacuated by a dry vacuum pump, and the degree of vacuum in the vacuum chamber is controlled to 10-5Magnitude. In the process, the vacuum degree detector can be used for monitoring the vacuum degree in the vacuum chamber in real time, so that the monitoring is more accurate.
And 102, adjusting the relative positions of the open X-ray machine, the single crystal and the detector to enable the center of an emergent port of the open X-ray machine, the center of an incident port of the detector and the center of the single crystal to be on the same horizontal plane.
In one particular process, X-rays emitted from an open X-ray machine are diffracted by a single crystal and then passed through a beryllium window in a vacuum chamber to be captured by a detector. Therefore, during the experiment, the positions of the open X-ray machine, the single crystal and the detector are accurately set. If the center of the exit port of the open X-ray machine, the center of the entrance port of the detector and the center of the single crystal are not in the same horizontal plane, especially when the center of the exit port of the open X-ray machine and the center of the entrance port of the detector are not in the same horizontal plane, no X-ray diffracted by the single crystal can be received by the detector if the angles of the single crystal and the incident X-ray are adjusted, so that the center of the exit port of the open X-ray machine, the center of the entrance port of the detector and the center of the single crystal need to be placed in the same horizontal plane, and the rotation adjustment processes of the open X-ray machine and the single crystal are both rotation on the same horizontal plane.
Specifically, the open type X-ray machine is started, X-rays are emitted, the single crystal is rotated in a gear linkage mode, the open type X-ray machine is rotated by a corresponding angle, the X-rays are diffracted on the single crystal to form a first diffraction angle, and the first monoenergetic X-rays are obtained after the X-rays are diffracted by the single crystal.
In addition, before the open type X-ray machine is started, the relative positions of the single crystal and the open type X-ray machine are adjusted in a gear linkage mode, namely, the positions of the single crystal and the open type X-ray machine are roughly adjusted.
In a specific process, before the open type X-ray machine is started, the positions of the single crystal and the open type X-ray machine are roughly adjusted, an angle between X-rays emitted by the open type X-ray machine and the single crystal is adjusted, so that the emergent direction of the X-rays after being diffracted by the single crystal is coincided with the X-ray receiving direction of the detector, the X-rays can be received by the detector, meanwhile, the angle between the single crystal and the emergent port direction of the open type X-ray machine is approximately a diffraction angle, and the experimental time is saved. And then, starting the open X-ray machine, emitting X-rays from an emergent port of the open X-ray machine to the single crystal, rotating the single crystal and the open X-ray machine respectively in a gear linkage mode, finely adjusting an angle between the single crystal and the emergent port of the open X-ray machine, and stopping rotating when the X-rays are diffracted on the single crystal.
And 104, emitting the first single-energy X-ray through a beryllium window of the vacuum chamber, and receiving the first single-energy X-ray by a detector.
In a specific process, first monoenergetic X-rays formed after diffraction by the crystal are emitted from a beryllium window of the vacuum chamber and are directly received by a detector. According to the adjusting method, the arrangement of the vacuum tube is reduced, the design is simple, the problem of high processing difficulty of the vacuum tube is solved, the mode that the open X-ray machine is combined with the vacuum chamber is adopted, the diffracted first monoenergetic X-ray passes through the beryllium window and is directly received by the detector, and the method is simple and easy to operate.
And 105, driving the single crystal and the open type X-ray machine to rotate in a gear linkage mode, forming a second diffraction angle between the X-ray and the single crystal, and forming a second mono-energy X-ray after the X-ray is diffracted by the single crystal.
Specifically, the driving dual gear drives the driven dual gear to rotate, the lower gear of the driven dual gear drives the single crystal to rotate by a first angle, and the upper gear of the driven dual gear drives the open type X-ray machine to rotate by a second angle corresponding to the first angle. Wherein, the upper gear and the lower gear of the driven double gear are connected through a rotary supporting structure.
In a specific in-process, the driving duplicate gear and the driven double gears are double gears, the upper gear and the lower gear of the driving duplicate gear are fixedly connected in the axial direction, the upper gear and the lower gear of the driven double gears are connected through the rotary supporting bearing, and therefore the upper gear and the lower gear of the driven double gears can independently rotate. Wherein, the last gear of driven double gear passes through the revolving stage and links to each other with open X-ray machine to when the last gear of driven double gear rotates, can drive open X-ray machine and rotate, simultaneously, the lower gear and the single crystal fixed connection of driven double gear drive the single crystal rotation when the lower gear of driven double gear rotates.
In order to generate Bragg diffraction, the up-down rotation speed ratio between the driving duplicate gear and the driven duplicate gear must be reasonably designed, so that on one hand, the experimental precision is ensured, on the other hand, the emergent direction of the X-ray emitted by the open X-ray machine after single crystal diffraction is unchanged, and the fixed detector can be always aligned to the emergent direction of the X-ray.
And 106, emitting the second single-energy X-ray through a beryllium window of the vacuum chamber, and receiving the second single-energy X-ray by a detector.
In a specific process, second monoenergetic X-rays formed after diffraction by the crystal are emitted from the beryllium window of the vacuum chamber and are directly received by the detector.
And step 107, changing an included angle between the X-ray and the single crystal to obtain the single-energy X-ray with different energies.
In a specific process, when different diffraction angles are formed between the X-ray and the single crystal, single-energy X-rays with different energies can be obtained. Therefore, in the experimental process, the angle between the X-rays emitted by the single crystal and the open X-ray machine is continuously changed in a gear linkage mode, so that different diffraction angles can be formed, and the single-energy X-rays with different energies can be obtained.
In this embodiment, the positions of the open X-ray machine, the single crystal, and the detector may be adjusted, and then the vacuum chamber is evacuated by the dry vacuum pump, when the vacuum degree reaches 10-5When Pa, the vacuum-pumping operation was stopped and the degree of vacuum in the vacuum chamber was controlled to 10-5Under the condition of magnitude, relative positions of the open X-ray machine, the single crystal and the detector are adjusted again, firstly, the center of an emergent port of the open X-ray machine, the center of an incident port of the detector and the center of the single crystal are ensured to be positioned on the same horizontal plane, a receiving port of the detector is in butt joint with a beryllium window of the vacuum chamber, then, the positions of the single crystal and the open X-ray machine are roughly adjusted in a gear linkage mode, so that a diffraction angle is formed between X-rays emitted by the single crystal and the open X-ray machine, the fine adjustment time is shortened, and the experiment time is saved. And then opening the open type X-ray machine, reducing the rotating speed of the driving duplicate gear, improving the adjustment precision, finely adjusting the positions of the single crystal and the open type X-ray machine, enabling an included angle between the single crystal and X-rays emitted by the open type X-ray machine to be a diffraction angle, namely the X-rays form diffraction on the single crystal, recording a first diffraction angle, and receiving the diffracted first monoenergetic X-rays by a detector. Then the angle between the X-rays emitted by the single crystal and the open X-ray machine is continuously changed in a gear linkage mode, and when different diffraction angles are formed, the single-energy X-rays with different energies can be obtained。
According to the adjusting method of the adjustable single crystal monochromator provided by the embodiment of the invention, a gear linkage mode is adopted, the driving gear and the driven gear both adopt double gears, two gears of the driven gear are connected by adopting a rotary supporting structure, the upper gear and the lower gear of the driven gear can be ensured to rotate independently, the upper gear drives the optical machine to rotate, the lower gear drives the single crystal to rotate, and the rotating speed ratio between the gears is reasonably designed, so that the included angle between the single crystal and incident X rays can be changed without changing the emergent direction of the X rays. Meanwhile, an open X-ray machine is adopted, so that the vacuum degree can be integrally controlled, and the signal intensity received by the detector is enhanced. The adjusting method is simple to operate and high in adjusting precision, and can control the adjusting precision by changing the rotating speed between the gears, so that errors are reduced.
Those of skill would further appreciate that the various illustrative components and algorithm steps described in connection with the embodiments disclosed herein may be implemented as electronic hardware, computer software, or combinations of both, and that the various illustrative components and steps have been described above generally in terms of their functionality in order to clearly illustrate this interchangeability of hardware and software. Whether such functionality is implemented as hardware or software depends upon the particular application and design constraints imposed on the implementation. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present invention.
The steps of a method or algorithm described in connection with the embodiments disclosed herein may be embodied in hardware, a software module executed by a processor, or a combination of the two. A software module may reside in Random Access Memory (RAM), memory, Read Only Memory (ROM), electrically programmable ROM, electrically erasable programmable ROM, registers, hard disk, a removable disk, a CD-ROM, or any other form of storage medium known in the art.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (4)
1. An adjustment method of an adjustable single crystal monochromator, the adjustment method comprising:
step A, carrying out vacuum pumping operation on a vacuum chamber by using a dry vacuum pump;
b, adjusting the relative positions of the open X-ray machine, the single crystal and the detector to enable the center of an emergent port of the open X-ray machine, the center of an incident port of the detector and the center of the single crystal to be positioned on the same horizontal plane;
step C, starting the open type X-ray machine, emitting X-rays, forming a first diffraction angle between the X-rays and the single crystal, and forming first monoenergetic X-rays after the X-rays are diffracted by the single crystal;
step D, the first single-energy X-ray is emitted through a beryllium window of the vacuum chamber and received by the detector;
step E, driving the single crystal and the open type X-ray machine to rotate in a gear linkage mode, forming a second diffraction angle between the X-ray and the single crystal, and forming a second mono-energy X-ray after the X-ray is diffracted by the single crystal;
step F, the second single-energy X-ray is emitted through a beryllium window of the vacuum chamber and received by the detector;
g, changing an included angle between the X-ray and the single crystal, and repeating the step E and the step F to obtain single-energy X-rays with different energies;
the step C specifically comprises the following steps:
starting the open X-ray machine to emit the X-ray;
rotating the single crystal in a gear linkage mode, and rotating the open type X-ray machine by a corresponding angle to diffract the X-rays on the single crystal to form a first diffraction angle;
obtaining a first monoenergetic X-ray after the X-ray is diffracted by the single crystal;
before the step C, the adjusting method further includes:
and adjusting the relative position of the single crystal and the open X-ray machine in a gear linkage mode.
2. The method of claim 1, wherein the vacuum chamber is at least 10 degrees f vacuum-5Magnitude.
3. The method of adjusting an adjustable monochromator according to claim 1, wherein rotating the single crystal and the open X-ray machine in a gear linkage manner, respectively, specifically comprises:
the driven double gears are driven to rotate through the driving duplicate gear;
the lower gear of the driven double gear drives the single crystal to rotate by a first angle;
and the upper gear of the driven double gear drives the open X-ray machine to rotate by a second angle corresponding to the first angle.
4. The method of adjusting an adjustable single crystal monochromator according to claim 3, wherein the upper gear and the lower gear of the driven dual gear are connected by a slewing support structure.
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| SU543858A1 (en) * | 1975-01-27 | 1977-01-25 | Ордена Трудового Красного Знамени Институт Кристаллографии Ан Ссср Им. А.В.Шубникова | Device for the study of the perfection of the structure of crystals |
| JPH0989813A (en) * | 1995-09-22 | 1997-04-04 | Rigaku Corp | Xafs measurement method and instrument |
| JP3813512B2 (en) * | 2002-01-07 | 2006-08-23 | 株式会社東芝 | Bonded substrate evaluation method and evaluation apparatus, and semiconductor device manufacturing method |
| CN1829910B (en) * | 2003-06-02 | 2012-05-23 | X射线光学系统公司 | Method and apparatus for implement XANES analysis |
| KR20050037086A (en) * | 2003-10-17 | 2005-04-21 | 삼성전자주식회사 | X-ray diffractometer and calibrating method of measuring position of the same |
| CN200944095Y (en) * | 2006-09-20 | 2007-09-05 | 北京逸东机电技术开发有限公司 | Light splitting and detecting device for rotary type bent crystal diffraction |
| JP5373660B2 (en) * | 2010-02-19 | 2013-12-18 | 日本電信電話株式会社 | Crystal structure analysis method |
| CN204789414U (en) * | 2015-06-29 | 2015-11-18 | 中国建材检验认证集团股份有限公司 | Provocative energy dispersion type X ray fluorescence appearance of single wavelength ray |
| CN107238620B (en) * | 2017-07-26 | 2023-03-24 | 中国地质大学（武汉） | X-ray fluorescence diffraction integrated analyzer of rotatable sample |
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