阅读说明：本技术 一种x射线发射低温荧光探测系统及方法 (X-ray emission low-temperature fluorescence detection system and method ) 是由 蔡碎女 刘良军 刘如海 于 2020-11-26 设计创作，主要内容包括：本发明涉及X射线领域,尤其涉及一种X射线发射低温荧光探测系统及方法。该系统包括工作台和固定在工作台上的射线发射调整装置和低温荧光探测装置；射线发射调整装置输出端与试样相对齐,并且射线发射调整装置输出端与射线接收装置输入端位于相同的衍射仪圆周上；低温荧光探测装置固定在工作台上,并且低温荧光探测装置输出端与试样相衔接；射线发射调整装置用于在衍射仪圆周上不同位置输出X射线；低温荧光探测装置用于探测接收试样受到X射线激发后产生的荧光；该部件通过设置射线发射调整装置减少对准试样时的累积误差,保证X射线和试样检测部位精确对准；通过设置低温荧光探测装置提高试样分析效率,保证试样检测后的质量。(The invention relates to the field of X-rays, in particular to an X-ray emission low-temperature fluorescence detection system and method. The system comprises a workbench, a ray emission adjusting device and a low-temperature fluorescence detection device, wherein the ray emission adjusting device and the low-temperature fluorescence detection device are fixed on the workbench; the output end of the ray emission adjusting device is aligned with the sample, and the output end of the ray emission adjusting device and the input end of the ray receiving device are positioned on the same circumference of the diffractometer; the low-temperature fluorescence detection device is fixed on the workbench, and the output end of the low-temperature fluorescence detection device is connected with the sample; the ray emission adjusting device is used for outputting X rays at different positions on the circumference of the diffractometer; the low-temperature fluorescence detection device is used for detecting fluorescence generated after the receiving sample is excited by X rays; the component reduces accumulated errors when aligning a sample by arranging a ray emission adjusting device, and ensures that X rays are accurately aligned with a sample detection part; the low-temperature fluorescence detection device is arranged to improve the analysis efficiency of the sample and ensure the quality of the detected sample.)

1. An X-ray emission low-temperature fluorescence detection system is characterized by comprising a workbench, a ray emission adjusting device (2) and a low-temperature fluorescence detection device (3), wherein the ray emission adjusting device and the low-temperature fluorescence detection device are fixed on the workbench; the output end of the ray emission adjusting device (2) is aligned with the sample, and the output end of the ray emission adjusting device (2) and the input end of the ray receiving device are positioned on the same circumference of the diffractometer; the low-temperature fluorescence detection device (3) is fixed on the workbench, and the output end of the low-temperature fluorescence detection device (3) is connected with the sample; the ray emission adjusting device (2) is used for outputting X rays at different positions on the circumference of the diffractometer; the low-temperature fluorescence detection device (3) is used for detecting fluorescence generated after the receiving sample is excited by X rays;

the low-temperature fluorescence detection device (3) comprises a receiving rack (31), a receiving driving mechanism (32) and a low-temperature fluorescence detection mechanism (33); the receiving rack (31) is fixed on the workbench, and the receiving driving mechanism (32) is fixed on the receiving rack (31); the output end of the receiving driving mechanism (32) is connected with the low-temperature fluorescence detection mechanism (33), and the output end of the low-temperature fluorescence detection mechanism (33) is connected with the sample; the receiving and driving mechanism (32) is used for driving the low-temperature fluorescence detection mechanism (33) to move to a detection station; the low-temperature fluorescence detection mechanism (33) is used for carrying out low-temperature treatment on the sample and detecting fluorescence generated after the sample is excited by X-rays.

2. An X-ray emission cryofluorescence detection system according to claim 1, characterized in that the radiation emission adjustment means (2) comprises an output drive mechanism (21), a radiation emission mechanism (22) and a radiation adjustment mechanism (23); the output driving mechanism (21) is fixed on the workbench, and the output end of the output driving mechanism (21) is respectively connected with the ray emitting mechanism (22) and the ray adjusting mechanism (23); the input end of the ray adjusting mechanism (23) is aligned with the output end of the ray emitting mechanism (22), and the output end of the ray adjusting mechanism (23) is aligned with the sample detection part; the output driving mechanism (21) is used for driving the ray emitting mechanism (22) and the ray adjusting mechanism (23) to move; a radiation emitting mechanism (22) for emitting X-rays; a radiation adjusting mechanism (23) for adjusting the irradiation position of the X-ray on the sample;

the ray adjusting mechanism (23) comprises an adjusting rack, a microscope (231), an adjusting driving assembly (232) and a collimator (233); the microscope (231) and the adjusting driving component (232) are fixed on the adjusting frame; the output end of the adjusting driving component (232) is connected with a collimator (233), and the collimator (233) is positioned between the output end of the microscope (231) and the sample; the microscope (231) objective comprises an objective hole, and X-rays emitted by the ray emission mechanism (22) pass through the objective hole, are collimated by the collimator (233) and then are aligned with the detection position of the sample; a microscope (231) for observing the position of the X-ray on the sample; the adjusting driving component (232) is used for adjusting the position of the collimator (233); the collimator (233) is used for focus collimation of the X-rays.

3. The X-ray emission cryofluorescence detection system of claim 2, wherein the adjustment drive assembly (232) comprises a first adjustment element (234) and a second adjustment element (235); the first adjusting element (234) is fixed on the adjusting frame, and the output end of the first adjusting element (234) is connected with the second adjusting element (235); the output end of the second adjusting element (235) is connected with the collimator (233);

the first adjusting element (234) comprises a horizontal micro-motion platform (2341) and a vertical micro-motion platform (2342); the output end of the horizontal micro-motion platform (2341) is connected with the vertical micro-motion platform (2342), and the output end of the vertical micro-motion platform (2342) is connected with the second adjusting element (235);

the horizontal micro-motion platform (2341) and the vertical micro-motion platform (2342) are both manually adjusted.

4. The X-ray emission cryofluorescence detection system of claim 3, wherein the second adjustment element (235) comprises a left-right rotation module (2351) and a front-back rotation module (2352); the output end of the left-right rotating module (2351) is connected with the front-back rotating module (2352), and the output end of the front-back rotating module (2352) is connected with the collimator (233); the left-right rotating module (2351) and the front-back rotating module (2352) are respectively used for driving the collimator (233) to rotate in the left-right direction and the front-back direction;

the output drive mechanism (21) comprises a first output drive (211) and a second output drive (212); the output end of the first output drive (211) is connected with the second output drive (212), and the output end of the second output drive (212) is connected with the adjusting rack; the first output drive (211) and the second output drive (212) are respectively used for driving the ray emission mechanism (22) to move in the horizontal direction and the vertical direction;

the first output drive (211) is a linear motor drive.

5. An X-ray emission cryofluorescence detection system according to claim 1, characterized in that the radiation emission modification device (2) further comprises a radiation absorbing mechanism (24); the ray absorption mechanism (24) is fixed on the adjusting machine frame, and the output end of the ray absorption mechanism (24) is connected with the part outside the detection part of the sample.

6. The X-ray emission cryofluorescence detection system of claim 5, wherein the radiation absorbing mechanism (24) comprises an absorption drive assembly (241) and an absorption fixture assembly (242); the output end of the absorption driving component (241) is connected with an absorption fixing component (242), and the absorption fixing component (242) is connected with the ray absorption block.

7. The X-ray emission cryofluorescence detection system of claim 1, wherein the cryofluorescence detection mechanism (33) comprises a detection base (331), a fluorescence detection cylinder (332), a fluorescence detector (333), a cryooutput cylinder (330), and a cryocooler (334); the detection bottom plate (331) is connected with the output end of the receiving driving mechanism (32), and the fluorescence detection cylinder (332) and the low-temperature output cylinder (330) are fixed on the detection bottom plate (331); the output end of the fluorescence detection cylinder (332) and the output end of the low-temperature output cylinder (330) are respectively connected with a fluorescence detector (333) and a low-temperature cooler (334), and the output end of the fluorescence detector (333) and the output end of the low-temperature cooler (334) are respectively connected with a sample; the fluorescence detector (333) is used for detecting fluorescence generated after the sample is excited by X rays; a cryocooler (334) is used to cryogenically process the sample.

8. The X-ray emission cryofluorescence detection system of claim 7, wherein the fluorescence detector (333) and cryocooler (334) are both angularly disposed and aligned with the sample;

the cooling medium of the low-temperature cooler (334) is liquid nitrogen;

the low-temperature fluorescence detection mechanism (33) further comprises a ray shielding component (335); the ray shielding component (335) is aligned with the output end of the ray emission adjusting device (2), and the ray shielding component (335) is positioned between the sample and an operator; the ray shielding component (335) is used for shielding redundant X rays output by the ray emission adjusting device (2);

the ray shielding assembly (335) comprises a shielding driving element (3351) and a shielding plate (3352); the shielding driving element (3351) is fixed on the detection bottom plate (331), and the output end of the shielding driving element (3351) is connected with the shielding plate (3352); the shielding plate (3352) is positioned at the rear side of the sample and is aligned with the output end of the ray emission adjusting device (2);

the shielding plate (3352) is in an inverted T shape, and the lower end of the inverted T shape of the shielding plate (3352) is connected with the rear side of the sample.

9. The X-ray emission cryofluorescence detection system of claim 8, wherein the shielding driving element (3351) comprises a shielding moving cylinder (3354) and a shielding rotating cylinder (3353); the shielding moving cylinder (3354) is fixed on the detection bottom plate (331), and the output end of the shielding moving cylinder (3354) is connected with the shielding rotating cylinder (3353); the output end of the shielding rotary cylinder (3353) is connected with a shielding plate (3352);

the receiving driving mechanism (32) comprises a receiving hand wheel (321), a receiving screw rod (322) and a receiving guide rail sliding block (323); the receiving hand wheel (321) is connected with the input end of the receiving screw rod (322), the output end of the receiving screw rod (322) is connected with the detection bottom plate (331), and the detection bottom plate (331) is connected with a slide block in the receiving guide rail slide block (323).

10. An X-ray emission low-temperature fluorescence detection method using an X-ray emission low-temperature fluorescence detection system according to claim 1, comprising the steps of:

x-ray emission adjustment: 1) the output driving mechanism (21) drives the ray adjusting mechanism (23) to move to the detection station; 2) observing the sample detection site through an eyepiece of a microscope (231), and adjusting the adjustment drive assembly (232) so that the output end of the collimator (233) is aligned with the sample detection site; 3) the X-ray emission mechanism (22) emits X-rays, the output driving mechanism (21) drives the output end of the X-ray emission adjusting device (2) to emit the X-rays at different incident angles relative to the detection position of the sample to detect the sample, and the X-ray receiving device receives the diffraction rays of the sample at a set position meeting the Bragg law to complete the X-ray emission adjusting process;

(II) low-temperature fluorescence detection: 1) installing the sample into a feeding device for positioning; 2) a receiving hand wheel (321) is rotated to adjust the low-temperature fluorescence detection mechanism (33) to move to a fluorescence detection station along a guide rail in a receiving guide rail sliding block (323); 3) the fluorescence detection cylinder (332) and the low-temperature output cylinder (330) respectively drive the fluorescence detector (333) and the cryocooler (334) to move downwards to a position connected with the sample; 4) the X-ray emission mechanism (22) emits X-rays to irradiate the sample, the low-temperature cooler (334) outputs a low-temperature medium to the sample, the ray receiving device carries out diffraction detection on the sample, and the fluorescence detector (333) carries out fluorescence detection on the sample to finish the low-temperature fluorescence detection process.

Technical Field

The invention relates to the field of X-rays, in particular to an X-ray emission low-temperature fluorescence detection system and method.

Background

The X-ray detection is based on the principle of diffraction, and when X-rays with known wavelength (characteristic X-rays with fixed wavelength are selected) are incident on a certain lattice plane with lattice spacing d of a lattice at a bragg angle, diffraction lines enhanced by superposition are obtained from a reflecting plane meeting the bragg condition. After the Bragg angle is measured, the space between the dot matrix planes, the unit cell size and the unit cell type can be determined by utilizing a Bragg formula, so that the phase analysis and the qualitative analysis are carried out on the sample.

The Chinese invention patent application (publication No. CN102435626A, published: 20120502) discloses a desk-top X-ray diffractometer, which comprises an X-ray generator, an angle measuring instrument, a high-voltage switch power supply and a control unit, wherein the angle measuring instrument is fixed on a rack through a base of the angle measuring instrument, the X-ray generator is fixedly arranged on an outer frame of the angle measuring instrument, and the high-voltage switch power supply is arranged in a bottom space of the rack; the goniometer is provided with a sample stage and a detector which are respectively connected with different driving devices; the ray receiving part of the detector rotates along with the reflection line of the X ray in the motion state, and the output signal of the goniometer is sent to the control unit. The invention adopts a table structure, solves the problems of large overall size and heat dissipation of the traditional X-ray diffractometer, reduces the energy consumption of a power supply, and is beneficial to energy conservation and emission reduction.

The prior art has the following defects: 1. when the X-ray detection position is aligned, firstly positioning a sample; then manually using the bottom surface of the tail end of the positioning die to contact and position the output end of the ray emission mechanism, and adjusting the collimator to align the collimator with the initial end of the positioning die to finish the alignment process of the X-ray detection position; the positioning mould has a certain manufacturing error, and a certain positioning error can be generated when the bottom surface of the tail end of the positioning mould is used as a positioning reference for positioning; when the collimator is adjusted to be aligned with the initial end of the positioning die, the alignment is adjusted through the size of human eyes, the accuracy of the size of the human eyes is lower relative to the X-ray detection size, and a larger observation error can be generated in the X-ray detection field by adjusting the collimator through the human eyes; the superposition of the positioning error generated by the positioning die and the observation error generated by the human eye adjusting collimator can cause that the accumulated error is larger when the X-ray is aligned with the detection part of the sample, which is not beneficial to the accurate alignment of the X-ray and the detection part of the sample. 2. When the sample is subjected to X-ray diffraction analysis to determine the spatial arrangement of atoms and fluorescence analysis to determine the types and the contents of elements, the sample is respectively arranged on diffraction analysis equipment and fluorescence analysis equipment to perform detection analysis so as to complete two analysis processes of the sample; when the diffraction analysis equipment and the fluorescence analysis equipment are separately detected, the sample needs to be positioned in the two equipment for two times respectively, so that the number of times of positioning the sample is increased, and the analysis efficiency of the sample is reduced; meanwhile, diffraction analysis equipment and fluorescence analysis are carried out on the sample at normal temperature, and the surface of the sample is easily damaged when the sample is subjected to X-ray irradiation at normal temperature; when a plurality of parts of the sample need to be subjected to X-ray diffraction analysis, the surface of the sample can be damaged in a large area, so that the quality of the sample after detection is not ensured.

Disclosure of Invention

The purpose of the invention is: aiming at the problems, the ray emission adjusting device is arranged to reduce the accumulated error when the sample is aligned, and ensure the accurate alignment of the X ray and the detection part of the sample; the X-ray emission low-temperature fluorescence detection system and the method improve the analysis efficiency of the sample and ensure the quality of the detected sample by arranging the low-temperature fluorescence detection device.

In order to achieve the purpose, the invention adopts the following technical scheme:

an X-ray emission low-temperature fluorescence detection system comprises a workbench, and a ray emission adjusting device and a low-temperature fluorescence detection device which are fixed on the workbench; the output end of the ray emission adjusting device is aligned with the sample, and the output end of the ray emission adjusting device and the input end of the ray receiving device are positioned on the same circumference of the diffractometer; the low-temperature fluorescence detection device is fixed on the workbench, and the output end of the low-temperature fluorescence detection device is connected with the sample; the ray emission adjusting device is used for outputting X rays at different positions on the circumference of the diffractometer; the low-temperature fluorescence detection device is used for detecting fluorescence generated after the receiving sample is excited by X rays; the low-temperature fluorescence detection device comprises a receiving rack, a receiving driving mechanism and a low-temperature fluorescence detection mechanism; the receiving machine frame is fixed on the workbench, and the receiving driving mechanism is fixed on the receiving machine frame; the output end of the receiving driving mechanism is connected with the low-temperature fluorescence detection mechanism, and the output end of the low-temperature fluorescence detection mechanism is connected with the sample; the receiving driving mechanism is used for driving the low-temperature fluorescence detection mechanism to move to a detection station; the low-temperature fluorescence detection mechanism is used for carrying out low-temperature treatment on the sample and detecting fluorescence generated after the sample is excited by X-rays.

Preferably, the ray emission adjusting device comprises an output driving mechanism, a ray emitting mechanism and a ray adjusting mechanism; the output driving mechanism is fixed on the workbench, and the output end of the output driving mechanism is respectively connected with the ray emitting mechanism and the ray adjusting mechanism; the input end of the ray adjusting mechanism is aligned with the output end of the ray emitting mechanism, and the output end of the ray adjusting mechanism is aligned with the sample detection part; the output driving mechanism is used for driving the ray emitting mechanism and the ray adjusting mechanism to move; the ray emission mechanism is used for emitting X rays; the X-ray adjusting mechanism is used for adjusting the irradiation position of the X-ray on the sample; the ray adjusting mechanism comprises an adjusting rack, a microscope, an adjusting driving assembly and a collimator; the microscope and the adjusting driving component are fixed on the adjusting rack; the output end of the adjusting driving assembly is connected with a collimator, and the collimator is positioned between the output end of the microscope and the sample; the microscope objective comprises an objective hole, and X rays emitted by the ray emission mechanism penetrate through the objective hole and are aligned with the detection position of the sample after being collimated by the collimator; the microscope is used for observing the position of the X-ray on the sample; the adjusting driving assembly is used for adjusting the position of the collimator; the collimator is used for performing focusing and collimation on the X-ray.

Preferably, the adjustment drive assembly comprises a first adjustment member and a second adjustment member; the first adjusting element is fixed on the adjusting rack, and the output end of the first adjusting element is connected with the second adjusting element; the output end of the second adjusting element is connected with the collimator; the first adjusting element comprises a horizontal micro-motion platform and a vertical micro-motion platform; the output end of the horizontal micro-motion platform is connected with the vertical micro-motion platform, and the output end of the vertical micro-motion platform is connected with the second adjusting element; the horizontal micro-motion platform and the vertical micro-motion platform are both manually adjusted.

Preferably, the second adjusting element comprises a left-right rotating module and a front-back rotating module; the output end of the left-right rotation module is connected with the front-back rotation module, and the output end of the front-back rotation module is connected with the collimator; the left-right rotating module and the front-back rotating module are respectively used for driving the collimator to rotate in the left-right direction and the front-back direction; the output driving mechanism comprises a first output drive and a second output drive; the first output drive output end is connected with the second output drive, and the second output drive output end is connected with the adjusting rack; the first output drive and the second output drive are respectively used for driving the ray emission mechanism to move in the horizontal direction and the vertical direction; the first output drive is a linear motor drive. The ray emission adjusting device also comprises a ray absorption mechanism; the ray absorption mechanism is fixed on the adjusting rack, and the output end of the ray absorption mechanism is connected with the part outside the detection part of the sample. The ray absorption mechanism comprises an absorption driving component and an absorption fixing component; the output end of the absorption driving component is connected with the absorption fixing component, and the absorption fixing component is connected with the ray absorption block.

Preferably, the low-temperature fluorescence detection mechanism comprises a detection bottom plate, a fluorescence detection cylinder, a fluorescence detector, a low-temperature output cylinder and a low-temperature cooler; the detection bottom plate is connected with the output end of the receiving driving mechanism, and the fluorescence detection cylinder and the low-temperature output cylinder are fixed on the detection bottom plate; the output end of the fluorescence detection cylinder and the output end of the low-temperature output cylinder are respectively connected with the fluorescence detector and the low-temperature cooler, and the output end of the fluorescence detector and the output end of the low-temperature cooler are respectively connected with the sample; the fluorescence detector is used for detecting fluorescence generated after the sample is excited by X rays; the cryocooler is used for carrying out low-temperature processing on the sample. The fluorescence detector and the cryocooler are distributed in an inclined mode, and the inclined angles are aligned with the sample; the cooling medium of the low-temperature cooler is liquid nitrogen; the low-temperature fluorescence detection mechanism also comprises a ray shielding assembly; the ray shielding assembly is aligned with the output end of the ray emission adjusting device and is positioned between the sample and an operator; the ray shielding component is used for shielding redundant X rays output by the ray emission adjusting device; the ray shielding assembly comprises a shielding driving element and a shielding plate; the shielding driving element is fixed on the detection bottom plate, and the output end of the shielding driving element is connected with the shielding plate; the shielding plate is positioned at the rear side of the sample and is aligned with the output end of the ray emission adjusting device; the shielding plate is in an inverted T shape, and the inverted T-shaped lower end of the shielding plate is connected with the rear side of the sample. The shielding driving element comprises a shielding moving cylinder and a shielding rotating cylinder; the shielding moving cylinder is fixed on the detection bottom plate, and the output end of the shielding moving cylinder is connected with the shielding rotating cylinder; the output end of the shielding rotary cylinder is connected with the shielding plate; the receiving driving mechanism comprises a receiving hand wheel, a receiving screw rod and a receiving guide rail slide block; the receiving hand wheel is connected with the input end of the receiving screw rod, the output end of the receiving screw rod is connected with the detecting bottom plate, and the detecting bottom plate is connected with a slide block in the receiving guide rail slide block.

In addition, the invention also discloses an X-ray emission low-temperature fluorescence detection method, which adopts the X-ray emission low-temperature fluorescence detection system and comprises the following steps:

x-ray emission adjustment: 1) the output driving mechanism drives the ray adjusting mechanism to move to a detection station; 2) observing the sample detection part through an eyepiece of the microscope, and adjusting the adjusting driving assembly to align the output end of the collimator with the sample detection part; 3) the ray emitting mechanism emits X rays, the output driving mechanism drives the output end of the ray emitting and adjusting device to emit the X rays at different incident angles relative to the detection position of the sample to detect the sample, and the ray receiving device receives the diffraction lines of the sample at the set position meeting the Bragg law to complete the sample ray output process;

(II) low-temperature fluorescence detection: 1) installing the sample into a feeding device for positioning; 2) rotating a receiving hand wheel, and adjusting the low-temperature fluorescence detection mechanism to move to a fluorescence detection station along a guide rail in a receiving guide rail slide block; 3) the fluorescence detection cylinder and the low-temperature output cylinder respectively drive the fluorescence detector and the low-temperature cooler to move downwards to a position connected with the sample; 4) the ray emitting mechanism emits X rays to irradiate the sample, the low-temperature cooler outputs a low-temperature medium to the sample, the ray receiving device performs diffraction detection on the sample, and the fluorescence detector performs fluorescence detection on the sample to complete the fluorescence receiving process of the sample.

The X-ray emission low-temperature fluorescence detection system and the method adopting the technical scheme have the advantages that:

1. by arranging a ray adjusting mechanism; after the ray adjusting mechanism moves to the detection station, observing the detection part of the sample through an eyepiece of the microscope, and adjusting the adjusting driving assembly to align the output end of the collimator with the detection part of the sample; the X-ray emission mechanism emits X-rays, the output driving mechanism drives the ray adjusting mechanism to emit the X-rays at different incident angles relative to the detection position of the sample to detect the sample, and the ray receiving device receives the diffraction rays of the sample at the set position meeting the Bragg law to complete the X-ray emission adjusting process. The alignment mode of the X-ray and the sample detection part is to perform positioning by observing through a microscope and then adjusting a collimator, and the positioning error is only derived from the observation error of the microscope; in addition, a positioning die is not needed in the positioning process, so that the positioning error caused by the manufacturing error of the positioning die and the like when the bottom surface of the positioning die is used as a positioning reference for positioning is avoided; when the microscope is used for observation, the detection position of the sample is amplified by multiple times, and the observation error is smaller than that of human eyes; the alignment mode only generates a small error of a microscope observation error, and avoids the accumulated error of superposition of the positioning error generated by the positioning mould and the observation error generated by the human eye adjusting collimator when the human eye observation positioning mould is aligned, thereby ensuring the accurate alignment of the X-ray and the sample detection part.

2. By arranging a low-temperature fluorescence detection mechanism. After the low-temperature fluorescence detection mechanism is adjusted to move to a fluorescence detection station, the fluorescence detection cylinder and the low-temperature output cylinder respectively drive the fluorescence detector and the cryocooler to move downwards to a position connected with the sample; the ray emitting mechanism emits X rays to irradiate the sample, the low-temperature cooler outputs a low-temperature medium to the sample, the ray receiving device carries out diffraction detection on the sample, and the fluorescence detector carries out fluorescence detection on the sample to complete the low-temperature fluorescence detection process. The low-temperature fluorescence detection mechanism simultaneously comprises a fluorescence detector and a low-temperature cooler; when the ray receiving device performs diffraction analysis on the sample, the cryocooler performs cooling treatment on the sample to protect the surface of the sample and reduce the damage of X rays on the sample, and the fluorescence detector also performs fluorescence analysis on the sample; namely, three analysis processes of diffraction analysis, low-temperature protection and fluorescence analysis of the sample can be completed simultaneously only by positioning the sample on the equipment once; therefore, the situation that the samples need to be disassembled and assembled for many times when different devices are used for analysis is avoided, and the analysis efficiency of the samples is improved.

Drawings

FIG. 1 is a schematic structural diagram of the present invention.

Fig. 2 is a schematic structural diagram of a ray emission adjusting device.

Fig. 3 is a schematic structural diagram of a ray adjustment mechanism.

Fig. 4 is a schematic structural view of the radiation absorbing mechanism.

Fig. 5 is a schematic structural diagram of the low-temperature fluorescence detection device.

Detailed Description

The following describes in detail embodiments of the present invention with reference to the drawings.

Example 1

An X-ray emission low-temperature fluorescence detection system as shown in FIG. 1 comprises a worktable, and a ray emission adjusting device 2 and a low-temperature fluorescence detection device 3 which are fixed on the worktable; the output end of the ray emission adjusting device 2 is aligned with the sample, and the output end of the ray emission adjusting device 2 and the input end of the ray receiving device are positioned on the same circumference of the diffractometer; the low-temperature fluorescence detection device 3 is fixed on the workbench, and the output end of the low-temperature fluorescence detection device 3 is connected with the sample; the ray emission adjusting device 2 is used for outputting X rays at different positions on the circumference of the diffractometer; the low-temperature fluorescence detection device 3 is used for detecting fluorescence generated after the receiving sample is excited by X-rays.

The product flow direction of the sample was: a radiation emission adjusting device 2 to a low temperature fluorescence detecting device 3.

As shown in fig. 2, the radiation emission adjusting device 2 includes an output driving mechanism 21, a radiation emitting mechanism 22, and a radiation adjusting mechanism 23; the output driving mechanism 21 is fixed on the workbench, and the output end of the output driving mechanism 21 is respectively connected with the ray emitting mechanism 22 and the ray adjusting mechanism 23; the input end of the ray adjusting mechanism 23 is aligned with the output end of the ray emitting mechanism 22, and the output end of the ray adjusting mechanism 23 is aligned with the sample detection part; the output driving mechanism 21 is used for driving the ray emitting mechanism 22 and the ray adjusting mechanism 23 to move; the radiation emitting mechanism 22 is used for emitting X-rays; the radiation adjustment mechanism 23 is used to adjust the irradiation position of the X-ray on the sample.

As shown in fig. 3, the ray adjustment mechanism 23 includes an adjustment gantry, a microscope 231, an adjustment drive assembly 232, and a collimator 233; the microscope 231 and the adjusting drive assembly 232 are both fixed on the adjusting frame; the output end of the adjustment driving assembly 232 is connected with a collimator 233, and the collimator 233 is positioned between the output end of the microscope 231 and the sample; the microscope 231 objective lens comprises an objective lens hole, and the X-ray emitted by the ray emission mechanism 22 passes through the objective lens hole and is aligned with the sample detection position after being collimated by the collimator 233; the microscope 231 is used to observe the position of the X-ray on the sample; the adjustment drive assembly 232 is used to adjust the position of the collimator 233; the collimator 233 is used for focus collimation of the X-rays. The adjustment drive assembly 232 includes a first adjustment member 234 and a second adjustment member 235; the first adjusting element 234 is fixed on the adjusting frame, and the output end of the first adjusting element 234 is connected with the second adjusting element 235; the output end of the second adjusting element 235 is connected with the collimator 233; first adjustment member 234 includes a horizontal micro platform 2341 and a vertical micro platform 2342; the output end of the horizontal micro-motion platform 2341 is connected with the vertical micro-motion platform 2342, and the output end of the vertical micro-motion platform 2342 is connected with the second adjusting element 235; the horizontal micro platform 2341 and the vertical micro platform 2342 are both manually adjustable. The second adjustment element 235 includes a left-right rotation module 2351 and a front-back rotation module 2352; the output end of the left-right rotating module 2351 is connected with the front-back rotating module 2352, and the output end of the front-back rotating module 2352 is connected with the collimator 233; the left-right rotating module 2351 and the front-back rotating module 2352 are used for driving the collimator 233 to rotate in the left-right direction and the front-back direction, respectively.

As shown in fig. 2, the output drive mechanism 21 includes a first output drive 211 and a second output drive 212; the output end of the first output driver 211 is connected with the second output driver 212, and the output end of the second output driver 212 is connected with the adjusting rack; the first output driver 211 and the second output driver 212 are respectively used for driving the ray emitting mechanism 22 to move in the horizontal direction and the vertical direction; the first output drive 211 is a linear motor drive. The radiation emission adjusting device 2 further comprises a radiation absorbing mechanism 24; the ray absorption mechanism 24 is fixed on the adjusting machine frame, and the output end of the ray absorption mechanism 24 is connected with the part outside the detection part of the sample.

As shown in fig. 4, the radiation absorbing mechanism 24 includes an absorption driving assembly 241 and an absorption fixing assembly 242; the output end of the absorption driving component 241 is connected with the absorption fixing component 242, and the absorption fixing component 242 is connected with the ray absorption block.

During operation of the radiation emission adjusting device 2: 1) the output driving mechanism 21 drives the ray adjusting mechanism 23 to move to the detection station; 2) observing the sample detection site through the eyepiece of the microscope 231, and adjusting the drive assembly 232 so that the output end of the collimator 233 is aligned with the sample detection site; 3) the ray emitting mechanism 22 emits X-rays, the output driving mechanism 21 drives the output end of the ray emitting and adjusting device 2 to emit X-rays at different incident angles relative to the detection position of the sample to detect the sample, and the ray receiving device receives the diffraction rays of the sample at the set position meeting the bragg law to complete the X-ray emitting and adjusting process.

The ray emission adjusting device 2 is used for positioning a sample when the X-ray detection position is aligned; then manually using the bottom surface of the tail end of the positioning die to contact and position the output end of the ray emission mechanism, and adjusting the collimator to align the collimator with the initial end of the positioning die to finish the alignment process of the X-ray detection position; the positioning mould has a certain manufacturing error, and a certain positioning error can be generated when the bottom surface of the tail end of the positioning mould is used as a positioning reference for positioning; when the collimator is adjusted to be aligned with the initial end of the positioning die, the alignment is adjusted through the size of human eyes, the accuracy of the size of the human eyes is lower relative to the X-ray detection size, and a larger observation error can be generated in the X-ray detection field by adjusting the collimator through the human eyes; the superposition of the positioning error generated by the positioning mould and the observation error generated by the human eye adjusting collimator can cause that the accumulated error is larger when the X-ray is aligned with the detection part of the sample, which is not beneficial to the accurate alignment of the X-ray and the detection part of the sample. By providing a ray adjustment mechanism 23; after the ray adjusting mechanism 23 moves to the detection station, observing the detection part of the sample through an eyepiece of a microscope 231, and adjusting the adjusting driving assembly 232 to align the output end of the collimator 233 with the detection part of the sample; the ray emitting mechanism 22 emits X-rays, the output driving mechanism 21 drives the ray adjusting mechanism 23 to emit X-rays at different incident angles relative to the sample detection position to detect the sample, and the ray receiving device receives the diffraction rays of the sample at the set position meeting the bragg law to complete the X-ray emission adjusting process. The alignment of the X-ray and the sample detection part is performed by observing through the microscope 231 and then adjusting the collimator 233, and the positioning error is only derived from the observation error of the microscope 231; in addition, a positioning die is not needed in the positioning process, so that the positioning error caused by the manufacturing error of the positioning die and the like when the bottom surface of the positioning die is used as a positioning reference for positioning is avoided; when the microscope 231 observes, the detection position of the sample is amplified by multiple times and then observed, and the observation error is smaller than that of human eyes; namely, the alignment mode only generates a small error such as a microscope 231 observation error, and avoids the accumulated error of superposition of the positioning error generated by the positioning mould and the observation error generated by the human eye adjusting collimator when the human eye observation positioning mould is aligned, thereby ensuring the accurate alignment of the X-ray and the sample detection part.

As shown in fig. 5, the low-temperature fluorescence detection device 3 includes a receiver frame 31, a receiving drive mechanism 32, and a low-temperature fluorescence detection mechanism 33; the receiver frame 31 is fixed on the workbench, and the receiving driving mechanism 32 is fixed on the receiver frame 31; the output end of the receiving driving mechanism 32 is connected with the low-temperature fluorescence detection mechanism 33, and the output end of the low-temperature fluorescence detection mechanism 33 is connected with the sample; the receiving and driving mechanism 32 is used for driving the low-temperature fluorescence detection mechanism 33 to move to a detection station; the low-temperature fluorescence detection mechanism 33 is used for carrying out low-temperature treatment on the sample and detecting fluorescence generated after the sample is excited by X-rays; the low-temperature fluorescence detection mechanism 33 comprises a detection bottom plate 331, a fluorescence detection cylinder 332, a fluorescence detector 333, a low-temperature output cylinder 330 and a low-temperature cooler 334; the detection bottom plate 331 is connected with the output end of the receiving driving mechanism 32, and the fluorescence detection cylinder 332 and the low-temperature output cylinder 330 are both fixed on the detection bottom plate 331; the output end of the fluorescence detection cylinder 332 and the output end of the low-temperature output cylinder 330 are respectively connected with a fluorescence detector 333 and a low-temperature cooler 334, and the output end of the fluorescence detector 333 and the output end of the low-temperature cooler 334 are respectively connected with a sample; the fluorescence detector 333 is used for detecting fluorescence generated after the sample is excited by X-rays; cryocooler 334 is used to cryogenically process the sample. The fluorescent detector 333 and the cryocooler 334 are both distributed in an inclined way, and the inclined angles are aligned with the sample; the cooling medium of cryocooler 334 is liquid nitrogen; the low-temperature fluorescence detection mechanism 33 further comprises a ray shielding component 335; the radiation shielding assembly 335 is aligned with the output of the radiation emission modification device 2 and the radiation shielding assembly 335 is positioned between the sample and the operator; the ray shielding component 335 is used for shielding the redundant X-rays output by the ray emission adjusting device 2; the ray shielding assembly 335 includes a shielding driving element 3351 and a shielding plate 3352; the shielding driving element 3351 is fixed on the detection base plate 331, and the output end of the shielding driving element 3351 is connected with the shielding plate 3352; the shielding plate 3352 is positioned at the rear side of the sample and is aligned with the output end of the radiation emission adjusting device 2; the shielding plate 3352 is in an inverted T shape, and the inverted T-shaped lower end of the shielding plate 3352 is connected with the rear side of the sample; the shielding driving element 3351 includes a shielding moving cylinder 3354 and a shielding rotating cylinder 3353; the shielding moving cylinder 3354 is fixed on the detection bottom plate 331, and the output end of the shielding moving cylinder 3354 is connected with the shielding rotating cylinder 3353; the output end of the shielding rotary cylinder 3353 is connected with the shielding plate 3352; the receiving driving mechanism 32 comprises a receiving hand wheel 321, a receiving screw rod 322 and a receiving guide rail slide block 323; the receiving hand wheel 321 is connected with the input end of the receiving screw rod 322, the output end of the receiving screw rod 322 is connected with the detection bottom plate 331, and the detection bottom plate 331 is connected with the slide block in the receiving guide rail slide block 323.

The low-temperature fluorescence detection device 3 is characterized in that in the working process: 1) installing a sample into the feeding device 1 for positioning; 2) rotating the receiving hand wheel 321 to adjust the low-temperature fluorescence detection mechanism 33 to move to the fluorescence detection station along the guide rail in the receiving guide rail sliding block 323; 3) the fluorescence detection cylinder 332 and the low-temperature output cylinder 330 respectively drive the fluorescence detector 333 and the low-temperature cooler 334 to move downwards to the position connected with the sample; 4) the radiation emitting mechanism 22 emits X-rays to irradiate the sample, the cryocooler 334 outputs a cryogenic medium to the sample, the radiation receiving device performs diffraction detection on the sample, and the fluorescence detector 333 performs fluorescence detection on the sample to complete the low-temperature fluorescence detection process.

The low-temperature fluorescence detection device 3 solves the problems that when the space arrangement of atoms and the type and content of elements are measured by the X-ray diffraction analysis and the fluorescence analysis of a sample, the sample is respectively arranged on diffraction analysis equipment and fluorescence analysis equipment to carry out detection and analysis, and two analysis processes of the sample are completed; when the diffraction analysis equipment and the fluorescence analysis equipment are separately detected, the sample needs to be positioned in the two equipment for two times respectively, so that the number of times of positioning the sample is increased, and the analysis efficiency of the sample is reduced; meanwhile, diffraction analysis equipment and fluorescence analysis are carried out on the sample at normal temperature, and the surface of the sample is easily damaged when the sample is subjected to X-ray irradiation at normal temperature; when a plurality of parts of the sample need to be subjected to X-ray diffraction analysis, the surface of the sample can be damaged in a large area, so that the quality of the detected sample is not ensured. By providing the low temperature fluorescence detection mechanism 33. After the low-temperature fluorescence detection mechanism 33 is adjusted to move to the fluorescence detection station, the fluorescence detection cylinder 332 and the low-temperature output cylinder 330 respectively drive the fluorescence detector 333 and the cryocooler 334 to move downwards to the position connected with the sample; the radiation emitting mechanism 22 emits X-rays to irradiate the sample, the cryocooler 334 outputs a cryogenic medium to the sample, the radiation receiving device performs diffraction detection on the sample, and the fluorescence detector 333 performs fluorescence detection on the sample to complete the low-temperature fluorescence detection process. The low-temperature fluorescence detection mechanism 33 simultaneously comprises a fluorescence detector 333 and a low-temperature cooler 334; when the ray receiving device performs diffraction analysis on the sample, the cryocooler 334 performs cooling treatment on the sample to protect the surface of the sample and reduce damage of the sample caused by X-rays, and the fluorescence detector 333 also performs fluorescence analysis on the sample; namely, three analysis processes of diffraction analysis, low-temperature protection and fluorescence analysis of the sample can be completed simultaneously only by positioning the sample on the equipment once; therefore, the situation that the samples need to be disassembled and assembled for many times when different devices are used for analysis is avoided, and the analysis efficiency of the samples is improved.