CN109490336B - Synchrotron radiation hard X-ray micro-focusing experimental method - Google Patents
Synchrotron radiation hard X-ray micro-focusing experimental method Download PDFInfo
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- CN109490336B CN109490336B CN201811348863.2A CN201811348863A CN109490336B CN 109490336 B CN109490336 B CN 109490336B CN 201811348863 A CN201811348863 A CN 201811348863A CN 109490336 B CN109490336 B CN 109490336B
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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
- G01N23/02—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 transmitting the radiation through the material
- G01N23/04—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 transmitting the radiation through the material and forming images of the material
- G01N23/043—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 transmitting the radiation through the material and forming images of the material using fluoroscopic examination, with visual observation or video transmission of fluoroscopic images
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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
Abstract
The invention relates to a synchrotron radiation hard X-ray micro-focusing experimental method, which comprises providing a synchrotron radiation hard X-ray micro-focusing experimental platform, wherein the platform comprises a focusing element which is arranged in sequence and used for receiving incident non-focusing hard X-rays and emitting focusing hard X-rays; a front ionization chamber assembly that limits the beam of the focused hard X-rays and measures the flux of the focused hard X-rays; a multi-dimensional sample console for adjusting the attitude of a sample placed thereon; the detector assembly is used for meeting the detection requirements of different experiments. The focusing element is combined with the specially-built front ionization chamber component, the multi-dimensional sample control table and the detector component, the posture of the sample is adjusted through the multi-dimensional sample control table, and the detection requirements of different experiments are met through the detector component, so that the requirements of performing fluorescence mapping experiments, microbeam diffraction experiments and microbeam absorption spectrum experiments on the sample in situ are met simultaneously.
Description
Technical Field
The invention relates to an optical experiment auxiliary device, in particular to a synchrotron radiation hard X-ray micro-focusing experiment method.
Background
The synchrotron radiation hard X-ray micro-focusing technology can focus hard X-rays on a micron or even submicron spatial scale so as to perform a series of researches with spatial resolution, wherein the hard X-ray micro-focusing experiments comprise fluorescence mapping experiments, microbeam diffraction experiments, microbeam absorption spectrum experiments and the like. The microbeam hard X-ray has higher spatial resolution capability, and can research the property difference of the sample at different spatial positions.
The existing micro-focusing experiment platforms are respectively optimized for the various experiment means, so that each experiment platform can only use one experiment method to represent the properties of a sample, namely, one experiment platform can only carry out one experiment on the same sample, and if various experiments are needed to be carried out on the same sample, the experiment can be realized by various different experiment platforms, for example, a fluorescence mapping experiment is carried out on a platform A, a diffraction experiment is carried out on a platform B, and a micro-beam absorption spectrum experiment is carried out on a platform C, the fluorescence mapping experiment requires that the sample and incident X-ray form an angle of 45 degrees, and the diffraction experiment requires that the sample is as perpendicular to the incident X-ray as possible; the diffraction experiment method requires that a surface detector is placed behind a sample, and an ionization chamber is placed behind the sample in an absorption spectrum experiment; the fluorescence mapping experiment requires stable position of the focused X-ray, and the absorption spectrum experiment requires energy conversion to cause the change of the position of the light spot, and the like. Therefore, if a plurality of different experiments are performed on the same platform, the illumination of the sample point in each experiment cannot be guaranteed to be the same.
Considering that in the current scientific research, a plurality of research methods are often needed to be used for comprehensively characterizing the properties of the same sample. At this moment, some problems will occur in the existing experimental platform, for example, some experimental methods cannot be used simultaneously, or the focusing hard X-ray cannot be guaranteed to be irradiated on the same position of the sample during use, so that the requirements of scientific research cannot be met.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a synchrotron radiation hard X-ray micro-focusing experimental method, so as to meet the requirements of performing fluorescence mapping experiment, micro-beam diffraction experiment and micro-beam absorption spectrum experiment on a sample in situ under the condition of meeting the hard X-ray micro-focusing experimental conditions.
The invention relates to a synchrotron radiation hard X-ray micro-focusing experimental method, which comprises the following steps:
step S0, providing a synchrotron radiation hard X-ray micro-focusing experimental platform, which comprises sequentially arranged:
a focusing element;
a front ionization chamber assembly for limiting the beam of the focused hard X-ray through a beam limiting hole and measuring the luminous flux of the focused hard X-ray;
a multi-dimensional sample console, comprising: a second Y-direction motor, a second X-direction motor, a second Z-direction motor, a first rotating motor, a third Y-direction motor, a third X-direction motor, a third Z-direction motor, a first pitch angle motor, a second rotating motor and a sample rack which are sequentially arranged together from bottom to top; and
a detector assembly, comprising: the system comprises a main control mobile motor, a manual Z-direction controller and a diffraction surface type detector which are sequentially arranged on the main control mobile motor from bottom to top, a rear ionization chamber bracket, a rear ionization chamber, a second pitch angle motor, a transfer plate, a translation motor and a fluorescence detector which are sequentially arranged on the main control mobile motor from bottom to top, and a fourth Z-direction motor, a fourth Y-direction motor and a microscope which are sequentially arranged on the main control mobile motor from bottom to top;
step S1, introducing the incident non-focused hard X-ray into the focusing element, and adjusting the focusing element to make the focusing element emit the focused hard X-ray;
step S2, calculating and obtaining the distance L between the beam limiting hole and the focusing point of the focused hard X-ray according to the cross section size and the focal length size of the unfocused hard X-ray and the aperture size of the beam limiting hole, and adjusting the relative position of the beam limiting hole and the focusing element according to the distance L;
step S3, adjusting the focused hard X-ray to pass through the center of the beam limiting hole;
step S4 of adjusting the second Y-direction motor, the second X-direction motor, and the second Z-direction motor so that the rotation shaft of the first rotation motor passes through the focus point of the focused hard X-ray;
step S5, placing a cross platinum wire on the sample rack;
step S6, adjusting the third Y-direction motor, the third X-direction motor, and the third Z-direction motor 308 so that the cross midpoint of the cross platinum wire is located at the focus point of the focused hard X-ray;
step S7, adjusting the main control mobile motor, the fourth Z-direction motor and the fourth Y-direction motor to enable the cross midpoint of the cross platinum wire to be aligned to the mark point on the focal plane of the microscope;
a step S8 of placing a sample on the sample holder;
step S9 of adjusting the first pitch angle motor so that the sample is parallel to the third Z-direction motor, and then adjusting the second rotating motor so that the sample is parallel to the third X-direction motor;
step S10, adjusting the third Y-direction motor, the third X-direction motor, and the third Z-direction motor to align the point of interest on the sample with a marker point on the focal plane of the microscope;
step S11, adjusting the main control mobile motor to place the fluorescence detector and the back ionization chamber on the light path;
step S12, adjusting the second pitch angle motor and the translation motor to enable the fluorescence detector to move in a direction forming an included angle of 30 degrees with the Y direction in a YZ plane until a preset angle and a preset distance are kept between the fluorescence detector and a point of interest on the sample;
step S13, scanning the third X-direction motor and the third Z-direction motor, and performing a fluorescence mapping experiment;
step S14, selecting an interest point on the sample to perform an absorption spectrum experiment according to an experiment result of a fluorescence mapping experiment and the luminous flux of the focused hard X-ray measured by the front ionization chamber component;
and step S15, adjusting the main control moving motor and the manual Z-direction controller to place the diffraction surface type detector at a preset position, and performing a micro-beam diffraction experiment on the point of interest on the sample.
In the above synchrotron radiation hard X-ray micro-focusing experimental method, the front ionization chamber assembly comprises:
a front ionization chamber base;
a first Y-direction motor mounted on the base of said front ionization chamber;
a first Z-direction motor mounted on the first Y-direction motor for moving along the Y direction under the driving of the first Z-direction motor;
a first X-direction motor mounted on the first Z-direction motor for movement in the Z-direction under the drive of the first Z-direction motor; and
and the front ionization chamber is connected with the first X-direction motor to move along the X direction under the driving of the first X-direction motor, and the front surface of the front ionization chamber is provided with the beam limiting hole.
In the above synchrotron radiation hard X-ray micro-focusing experimental method, the multi-dimensional sample console further comprises: and the console base is used for mounting the second Y-direction motor on the console base.
In the above synchrotron radiation hard X-ray micro-focusing experimental method, the detector assembly further includes: and the detector base is used for mounting the main control mobile motor on the detector base.
In the above synchrotron radiation hard X-ray micro-focusing experimental method, the focusing element is a KB mirror, a zone plate or a compound refractive lens.
In the above synchrotron radiation hard X-ray micro-focusing experimental method, the step S2 further includes: firstly, the microscope is focused on the focusing element, then the fourth Y-direction motor is adjusted to enable the microscope to move for 2L along the Y direction, and then the first Y-direction motor is adjusted to enable the beam limiting hole to appear on the focal plane of the microscope.
In the above synchrotron radiation hard X-ray micro-focusing experimental method, the step S2 further includes: the center of the beam limiting hole firstly passes through the optical path, then the beam limiting hole is moved to the focusing element, and the reading change of the rear ionization chamber is observed, and when the reading just begins to descend, the position of the beam limiting hole is determined.
In the above-mentioned synchrotron radiation hard X-ray micro-focusing experimental method, in step S14, if the mass content of the element of interest in the sample is less than 1%, a fluorescence absorption spectrum experiment is directly performed by the fluorescence detector, and if the mass content of the element of interest in the sample is greater than 1%, the translation motor is adjusted to make the fluorescence detector 5mm-100mm away from the sample, and a fluorescence absorption spectrum experiment is performed, or a transmission absorption spectrum experiment is performed by the back ionization chamber.
Due to the adoption of the technical scheme, the focusing element is combined with the specially-built front ionization chamber component, the multi-dimensional sample control table and the detector component, the posture of the sample is adjusted through the multi-dimensional sample control table, and the detection requirements of different experiments are met through the detector component, so that the requirements of carrying out fluorescence mapping experiments, microbeam diffraction experiments and microbeam absorption spectrum experiments on the sample in situ are met simultaneously.
Drawings
FIG. 1 is a schematic diagram illustrating the definition of various directions involved in a synchrotron radiation hard X-ray micro-focusing experimental method of the present invention;
FIG. 2 is a schematic structural diagram of a synchrotron radiation hard X-ray micro-focusing experimental method of the present invention;
FIG. 3 is a schematic structural diagram of a front ionization chamber assembly in a synchrotron radiation hard X-ray micro-focusing experimental method of the present invention;
FIG. 4 is a schematic structural diagram of a multi-dimensional sample console in the synchrotron radiation hard X-ray micro-focusing experimental method of the present invention;
FIG. 5 is a schematic structural diagram of a detector assembly in the synchrotron radiation hard X-ray micro-focusing experimental method of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
As shown in fig. 1, since X-rays of a general synchrotron radiation device propagate in a horizontal plane, a direction along the X-ray propagation direction (i.e., an optical path propagation direction) is defined as a Y-direction, a horizontal direction perpendicular to the optical path propagation direction is defined as an X-direction, a vertical direction perpendicular to a horizontal plane is defined as a Z-direction, a pitch along the optical path propagation direction is defined as a pitch direction, a rotation in the horizontal plane is defined as a rotation direction, and an inclination perpendicular to the optical path propagation direction is defined as an inclination direction.
As shown in fig. 2, the present invention, i.e. a synchrotron radiation hard X-ray micro-focusing experimental method, includes the following steps:
step S0, providing a synchrotron radiation hard X-ray micro-focusing experiment platform, as shown in fig. 2, the experiment platform comprises a focusing element 1, a front ionization chamber assembly 2, a multi-dimensional sample console 3 and a detector assembly 4, which are arranged in sequence, wherein,
the focusing element 1 is used for receiving incident unfocused hard X-rays (incident from left to right in fig. 2) and emitting focused hard X-rays, and may be a KB mirror (Kirkpatrick-Baez mirror), a zone plate, a compound refractive lens, or the like (in this embodiment, a KB mirror);
the front ionization chamber assembly 2 is used for limiting the beam of the focused hard X-ray emitted from the focusing element 1 and measuring the luminous flux of the focused hard X-ray;
the multi-dimensional sample control platform 3 is used for adjusting the posture of a sample placed on the multi-dimensional sample control platform and calibrating the distance between the detector assembly 4 and the sample;
the detector assembly 4 is used for calibrating the position of a sample and meeting the detection requirements of different experiments.
As shown in fig. 3, the front ionization chamber assembly 2 specifically includes:
a front ionization chamber base 201;
a first Y-direction motor 202 mounted on the front ionization chamber base 201;
a first Z-direction motor 203 mounted on the first Y-direction motor 202 to move in the Y-direction by being driven by the first Z-direction motor;
a first X-direction motor 204 mounted on the first Z-direction motor 203 to move in the Z-direction by being driven by the first Z-direction motor; and
and a front ionization chamber 205 connected to the first X-direction motor 204 to move in the X-direction by being driven, and having a front surface provided with a beam-limiting hole 206.
When the focused hard X-rays generated by the focusing element 1 pass through the front ionization chamber assembly 2, the beam limiting hole 206 limits the beam of the focused hard X-rays, so that stray light is shielded, and the focal points of the focused hard X-rays at different energies are kept consistent. The confined focused hard X-rays enter the front ionization chamber 205, and their flux is tested by the front ionization chamber 205. Because the focused hard X-rays tested by the front ionization chamber 205 do not contain stray light and the front ionization chamber is very close to the sample point on the sample on the multidimensional sample console 3, the incident luminous flux tested by the front ionization chamber is very accurate, thereby being beneficial to quantitatively analyzing the mass content of each element of interest in a fluorescence mapping experiment and obtaining high-precision absorption spectrum data.
As shown in fig. 4, the multi-dimensional sample console 3 specifically includes:
a console base 301;
a second Y-direction motor 302 mounted on the console base 31;
a second X-direction motor 303 mounted on the second Y-direction motor 302 to be moved in the Y-direction by being driven thereby;
a second Z-direction motor 304 mounted on the second X-direction motor 303 to move in the X-direction by being driven by the second Z-direction motor;
a first rotary motor 305 mounted on the second Z-direction motor 304 to be moved in the Z-direction by being driven thereby;
a third Y-direction motor 306 mounted on the first rotating motor 305 to be moved in a rotating direction by being driven by it;
a third X-direction motor 307 mounted on the third Y-direction motor 306 to move in the Y-direction by being driven by the same;
a third Z-direction motor 308 mounted on the third X-direction motor 307 to be moved in the X-direction by being driven;
a first pitch angle motor 309 mounted on the third Z-direction motor 308 to be moved in the Z-direction by being driven thereby;
a second rotating motor 310 mounted on the first pitch angle motor 309 to be moved in a pitch direction by being driven by the same; and
and a sample holder 311 mounted on the second rotary motor 310 to be moved in a rotational direction by the second rotary motor, for placing a sample thereon.
The above-mentioned multidimensional sample control platform 3 has a rotation center calibration function, wherein:
the lowermost second Y-direction motor 302, second X-direction motor 303, and second Z-direction motor 304 are used to implement X, Y, Z three-directional dimensional adjustment of the entire console attitude, where the second Y-direction motor 302 and second X-direction motor 303 as translation motors can align the vertical-direction rotation axis of the first rotation motor 305 to the focal point of the focused hard X-rays emitted from the front ionization chamber 205 (i.e., the focused hard X-rays are finally focused to one point after being emitted from the front ionization chamber 205), the second Z-direction motor 304 as an auxiliary axis, or compensate the height of the sample when it is too short and the third Z-direction motor 308 cannot move the sample onto the optical path; before the experiment, the second Y-direction motor 302, the second X-direction motor 303 and the second Z-direction motor 304 need to be adjusted in advance and kept still during the experiment;
the third Y-direction motor 306, the third X-direction motor 307 and the third Z-direction motor 308 in the middle part are used as sample adjusting motors to respectively realize X, Y, Z three-direction dimension adjustment of sample postures in experiments, so that the sample points of interest are moved to the focus points of focused hard X-rays, the spatial resolution capability of the focused hard X-rays can be optimally utilized, the distance between the sample points of interest and the detector assembly is ensured to be consistent, the distance consistency is ensured to be the key for collecting high-precision diffraction data and fluorescence data, the motors in the middle parts can collect experimental data for different positions of the samples by scanning, and the key of the focused hard X-ray experiments is located;
the uppermost first pitch motor 309 and second rotation motor 310 are used to calibrate the sample in the rotation and pitch directions when the sample is placed on the sample holder 311, this is because the sample is usually fixed on the sample holder by glue or a clamp, which inevitably causes the sample not to completely adhere to the sample holder, when the sample is scanned by the motor in the middle, the non-fitting degree brings errors, and can cause errors of experimental data when the non-fitting degree is serious, the first pitch angle motor 309 and the second rotation motor 310, therefore, calibrate the sample attitude in two dimensions, the sample can be made completely parallel to the scan direction of the motor in the middle, thus to neutralize the above errors, it should be noted that the same sample is calibrated only once before the experiment, and the first pitch angle motor 309 and the second rotating motor 310 will remain stationary after calibration, and the change of the sample angle is realized by the first rotating motor 305 during the experiment.
As shown in fig. 5, the detector assembly 4 specifically includes:
a probe mount 401;
a main control moving motor 402 mounted on the probe base 401;
a manual Z-direction controller 403 mounted on the main control moving motor 402 to move in the X-direction by being driven by the same;
a diffraction surface type detector 404 mounted on the manual Z-direction controller 403 to move in the Z-direction by being driven by the same;
a rear ionization chamber support 405 mounted on the main control moving motor 402 to move in the X direction by being driven by the main control moving motor;
a rear ionization chamber 406 mounted on rear ionization chamber mount 405, which is supported by rear ionization chamber mount 405 onto the optical path;
a second pitch motor 407 mounted on the rear ionization chamber 406;
a translation motor 409 which is arranged on the second pitch angle motor 407 through an adapter plate 408 and driven by the second pitch angle motor to move along the pitch direction until an included angle of 30 degrees is formed between the translation motor and the Y direction;
a fluorescence detector 410 mounted on the translation motor 409 to move in a direction forming an included angle of 30 degrees with the Y direction in the YZ plane under the driving of the translation motor;
a fourth Z-direction motor 411 installed on the main control moving motor 402 to move in the X-direction by being driven by the same;
a fourth Y-direction motor 412 mounted on the fourth Z-direction motor 411 to be moved in the Z-direction by being driven; and
and a microscope 413 mounted on the fourth Y-direction motor 412 to be moved in the Y-direction by being driven by the same.
The main control moving motor 402 can move the diffraction surface type detector 404, the rear ionization chamber 406, the fluorescence detector 410 and the microscope 413 placed thereon to the optical path according to different experimental stages. Specifically, the sample is placed perpendicular to the optical path, the microscope 413 is used for calibrating a focusing point for focusing the hard X-ray before the experiment, and is used for assisting in placing an interest point on the sample (the interest point is a spatial point where the focusing point for focusing the hard X-ray and the sample are overlapped, the point on the sample is irradiated by the X-ray to generate various effects, and the observation of the effects is an X-ray experiment) on the focusing point, because the microscope 413 is placed along the optical path direction, compared with the existing experiment platform in which the microscope is placed at an angle of 45 degrees with the optical path in the front ionization chamber, the focusing point calibrated by the microscope 413 is more accurate, and therefore, errors caused by the focal depth of the microscope cannot exist; when the experiment is started, the microscope 413 is moved out of the optical path, and then the diffraction surface type detector 404, the rear ionization chamber 406 and the fluorescence detector 410 are moved into the optical path as required.
In addition, the focusing element 1 is a conventional device, and the positions of the front ionization chamber assembly 2, the multi-dimensional sample console 3 and the detector assembly 4 can be located according to the characteristics of the focusing element 1, for example, if the half height width of incident X-ray of the focusing element 1 is S, the focal length is d, and the aperture of the beam limiting hole 206 of the front ionization chamber assembly 2 is 50 micrometers, the distance from the front surface of the front ionization chamber 205 to the focusing element 1 is (1-50/S) × d, for example, the diameter of the cross section of incident X-ray is 500 micrometers, the focal length is 30 centimeters, and the diameter of the beam limiting hole 206 is 100 micrometers, the distance from the beam limiting hole 206 to the focusing point should be 10 centimeters; the distance from the center of the multi-dimensional sample control platform 3 to the focusing element 1 is d; the distance of the detector assembly 4 from the centre of the multi-dimensional sample console 3 is determined according to the sample properties.
Based on the synchrotron radiation hard X-ray micro-focusing experimental platform, the experimental method provided by the invention further comprises the following steps of:
step S1, introducing the incident non-focusing hard X-ray into the focusing element 1, and adjusting the focusing element 1 to make the emergent light thereof be focusing hard X-ray;
step S2, calculating a distance L from the beam limiting hole 206 to the focal point of the focused hard X-ray according to the cross-sectional size and the focal length size of the incident unfocused hard X-ray and the aperture size of the beam limiting hole 206 of the front ionization chamber 25, and adjusting the position of the beam limiting hole 206 by the first Y-direction motor 202 according to the distance L;
step S3, adjusting the first Z-direction motor 203 and the first X-direction motor 204 so that the focused hard X-rays pass through the center of the beam limiting aperture 206;
step S4 of adjusting the second Y-direction motor 302, the second X-direction motor 303, and the second Z-direction motor 304 so that the rotation axis of the first rotation motor 305 passes through the focus point of the focused hard X-rays;
step S5, placing a cross platinum wire (not shown) on the sample holder 311;
step S6, adjusting the third Y-direction motor 306, the third X-direction motor 307, and the third Z-direction motor 308 so that the cross midpoint of the cross platinum wire is located at the focus point of the focused hard X-rays;
step S7, adjusting the main control moving motor 402, the fourth Z-direction motor 411, and the fourth Y-direction motor 412 to align the cross midpoint of the cross platinum wire with a marker point (which is used to assist in calibrating the position of the point of interest on the sample) on the focal plane of the microscope 413;
step S8, placing the sample on the sample holder 311;
step S9, adjusting the first pitch angle motor 309 so that the sample is parallel to the third Z direction motor 308, and then adjusting the second rotation motor 310 so that the sample is parallel to the third X direction motor 307;
step S10, adjusting the third Y-direction motor 306, the third X-direction motor 307, and the third Z-direction motor 308 to align the point of interest on the sample with the marker point on the focal plane of the microscope 413;
step S11, adjusting master moving motor 402 to place fluorescence detector 410 and back ionization chamber 406 on the light path;
step S12, adjusting the second pitch angle motor 407 and the translation motor 409 to make the fluorescence detector 410 move in the YZ plane at an angle of 30 ° with the Y direction until keeping a suitable angle and distance (e.g., angle range of 30 ± 5 ° and distance range of 5-100mm) with the point of interest on the sample;
step S13, scanning the third X-direction motor 307 and the third Z-direction motor 308, and performing a fluorescence mapping experiment;
step S14, according to the experiment result of the fluorescence mapping experiment and the flux of the focused hard X-ray measured by the front ionization chamber component 2, selecting the point of interest on the sample to perform the absorption spectrum experiment, wherein if the mass content of the element of interest in the sample is low (the content is determined according to the measurement of the front ionization chamber component, for example, less than 1%), the fluorescence absorption spectrum experiment is directly performed through the fluorescence detector, and if the mass content of the element of interest in the sample is high (for example, more than 1%), the translation motor 409 is adjusted to make the fluorescence detector 413 far away from the sample (for example, the distance between the fluorescence detector and the sample is 5mm-100 mm; the range is determined by the travel of the translation motor), the receiving solid angle is reduced, the fluorescence absorption spectrum experiment is performed, or the transmission absorption spectrum experiment is performed through the rear ionization chamber 406;
step S15, the master control moving motor 402 and the manual Z-direction controller 403 are adjusted to place the diffraction surface detector 404 at a proper position (under the condition that the through X-rays are irradiated on the detector, the specific position of the diffraction surface detector 404 is determined according to the diffraction fringes of the sample, so as to make the diffraction fringes required to be detected fall on the diffraction surface detector 404 as much as possible), thereby performing the microbeam diffraction experiment on the point of interest.
In the above step S2, the position of the beam-defining aperture 206 may also be determined with the aid of the microscope 413: first, the microscope 413 is focused on the focusing element 1, then the fourth Y-direction motor 412 is adjusted to move the microscope 413 by a distance of 2L in the Y-direction, and then the first Y-direction motor 202 is adjusted to make the beam limiting hole 206 appear on the focal plane of the microscope 413, thereby ensuring that the distance between the beam limiting hole 206 and the focal point of the focused hard X-rays is L.
Alternatively, in step S2, the position of the beam limiting aperture 206 may also be determined by the back ionization chamber 406: firstly, the center of the beam limiting hole 206 is ensured to pass through the optical path, then the beam limiting hole 206 is slowly moved to the focusing element 1, and the reading change of the rear ionization chamber 406 is observed, and when the reading just begins to descend, the position of the beam limiting hole 206 is a theoretically proper position.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (8)
1. A synchrotron radiation hard X-ray micro-focusing experimental method is characterized by comprising the following steps:
step S0, providing a synchrotron radiation hard X-ray micro-focusing experimental platform, which comprises sequentially arranged:
a focusing element for receiving incident unfocused hard X-rays and emitting focused hard X-rays;
a front ionization chamber assembly for limiting the beam of the focused hard X-ray through a beam limiting hole and measuring the luminous flux of the focused hard X-ray;
a multi-dimensional sample console, comprising: a second Y-direction motor, a second X-direction motor, a second Z-direction motor, a first rotating motor, a third Y-direction motor, a third X-direction motor, a third Z-direction motor, a first pitch angle motor, a second rotating motor and a sample rack which are sequentially arranged together from bottom to top; and
a detector assembly, comprising: the system comprises a main control mobile motor, a manual Z-direction controller and a diffraction surface type detector which are sequentially arranged on the main control mobile motor from bottom to top, a rear ionization chamber bracket, a rear ionization chamber, a second pitch angle motor, a transfer plate, a translation motor and a fluorescence detector which are sequentially arranged on the main control mobile motor from bottom to top, and a fourth Z-direction motor, a fourth Y-direction motor and a microscope which are sequentially arranged on the main control mobile motor from bottom to top;
step S1, introducing the incident non-focused hard X-ray into the focusing element, and adjusting the focusing element to make the focusing element emit the focused hard X-ray;
step S2, calculating and obtaining the distance L between the beam limiting hole and the focusing point of the focused hard X-ray according to the cross section size and the focal length size of the unfocused hard X-ray and the aperture size of the beam limiting hole, and adjusting the relative position of the beam limiting hole and the focusing element according to the distance L;
step S3, adjusting the focused hard X-ray to pass through the center of the beam limiting hole;
step S4 of adjusting the second Y-direction motor, the second X-direction motor, and the second Z-direction motor so that the rotation shaft of the first rotation motor passes through the focus point of the focused hard X-ray;
step S5, placing a cross platinum wire on the sample rack;
step S6, adjusting the third Y-direction motor, the third X-direction motor and the third Z-direction motor to enable the cross midpoint of the cross platinum wire to be positioned on the focusing point of the focused hard X-ray;
step S7, adjusting the main control mobile motor, the fourth Z-direction motor and the fourth Y-direction motor to enable the cross midpoint of the cross platinum wire to be aligned to the mark point on the focal plane of the microscope;
a step S8 of placing a sample on the sample holder;
step S9 of adjusting the first pitch angle motor so that the sample is parallel to the third Z-direction motor, and then adjusting the second rotating motor so that the sample is parallel to the third X-direction motor;
step S10, adjusting the third Y-direction motor, the third X-direction motor, and the third Z-direction motor to align the point of interest on the sample with a marker point on the focal plane of the microscope;
step S11, adjusting the main control mobile motor to place the fluorescence detector and the back ionization chamber on the light path;
step S12, adjusting the second pitch angle motor and the translation motor to enable the fluorescence detector to move in a direction forming an included angle of 30 degrees with the Y direction in a YZ plane until a preset angle and a preset distance are kept between the fluorescence detector and a point of interest on the sample;
step S13, scanning the third X-direction motor and the third Z-direction motor, and performing a fluorescence mapping experiment;
step S14, selecting an interest point on the sample to perform an absorption spectrum experiment according to an experiment result of a fluorescence mapping experiment and the luminous flux of the focused hard X-ray measured by the front ionization chamber component;
and step S15, adjusting the main control moving motor and the manual Z-direction controller to place the diffraction surface type detector at a preset position, and performing a micro-beam diffraction experiment on the point of interest on the sample.
2. The synchrotron hard X-ray microfocus experimental method of claim 1, wherein the front ionization chamber assembly comprises:
a front ionization chamber base;
a first Y-direction motor mounted on the base of said front ionization chamber;
a first Z-direction motor mounted on the first Y-direction motor for moving along the Y direction under the driving of the first Z-direction motor;
a first X-direction motor mounted on the first Z-direction motor for movement in the Z-direction under the drive of the first Z-direction motor; and
and the front ionization chamber is connected with the first X-direction motor to move along the X direction under the driving of the first X-direction motor, and the front surface of the front ionization chamber is provided with the beam limiting hole.
3. The synchrotron hard X-ray microfocus experimental method of claim 1, wherein the multi-dimensional sample console further comprises: and the console base is used for mounting the second Y-direction motor on the console base.
4. The synchrotron hard X-ray microfocus experimental method of claim 1, wherein the detector assembly further comprises: and the detector base is used for mounting the main control mobile motor on the detector base.
5. The synchrotron radiation hard X-ray microfocus experimental method of claim 1, wherein the focusing element is a KB mirror, a zone plate, or a compound refractive lens.
6. The synchrotron hard X-ray microfocus experimental method of claim 2, wherein said step S2 further comprises: firstly, the microscope is focused on the focusing element, then the fourth Y-direction motor is adjusted to enable the microscope to move for 2L along the Y direction, and then the first Y-direction motor is adjusted to enable the beam limiting hole to appear on the focal plane of the microscope.
7. The synchrotron hard X-ray microfocus experimental method of claim 1, wherein said step S2 further comprises: the center of the beam limiting hole firstly passes through the optical path, then the beam limiting hole is moved to the focusing element, and the reading change of the rear ionization chamber is observed, and when the reading just begins to descend, the position of the beam limiting hole is determined.
8. The method of claim 1, wherein in step S14, if the mass content of the element of interest in the sample is less than 1%, the fluorescence absorption spectroscopy experiment is performed directly by the fluorescence detector, and if the mass content of the element of interest in the sample is greater than 1%, the translation motor is adjusted to make the fluorescence detector 5mm-100mm away from the sample, and the fluorescence absorption spectroscopy experiment is performed, or the transmission absorption spectroscopy experiment is performed by the back ionization chamber.
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