CN103175857A - Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device - Google Patents

Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device Download PDF

Info

Publication number
CN103175857A
CN103175857A CN2013100816138A CN201310081613A CN103175857A CN 103175857 A CN103175857 A CN 103175857A CN 2013100816138 A CN2013100816138 A CN 2013100816138A CN 201310081613 A CN201310081613 A CN 201310081613A CN 103175857 A CN103175857 A CN 103175857A
Authority
CN
China
Prior art keywords
lifting
slit
ray
sample
detector
Prior art date
Application number
CN2013100816138A
Other languages
Chinese (zh)
Other versions
CN103175857B (en
Inventor
谢亚宁
张静
张久昶
宋冬燕
Original Assignee
中国科学院高能物理研究所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 中国科学院高能物理研究所 filed Critical 中国科学院高能物理研究所
Priority to CN201310081613.8A priority Critical patent/CN103175857B/en
Publication of CN103175857A publication Critical patent/CN103175857A/en
Application granted granted Critical
Publication of CN103175857B publication Critical patent/CN103175857B/en

Links

Abstract

The invention discloses a device specially used for a grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and a regulating method of the device. The device comprises a device for generating an X ray required by the grazing incidence XAFS experiment, a front slit for defining the size of the X ray, a first lifting platform for enabling the front slit to go up and down in the vertical direction, a sample frame for bearing a sample, a rotating platform for rotating the sample on the sample frame to obtain the required X ray grazing incidence angle, a second lifting platform for enabling the rotating platform to go up and down in the vertical direction, a rear slit for limiting the size of a total-reflection X ray, a third lifting platform for enabling the rear slit to go up and down in the vertical direction, a first detector for detecting a fluorescence signal sent by the sample, and a second detector for detecting a total-reflection X ray signal. By adopting the device and method, the initial position of the sample can be rapidly and accurately set, the sample angle can be accurately regulated, experimental detection data of the sample can be obtained at high signal to noise ratio, and a high-quality grazing incidence XAFS experiment spectrum is acquired.

Description

Be exclusively used in device and the method for adjustment thereof of glancing incidence XAFS experiment
Technical field
The present invention relates to modern structure of matter analytical approach-synchrotron radiation experimental technique, particularly relate to a kind of device of glancing incidence X ray Absorption Fine Structure (X-ray Absorption Fine Structure, XAFS) experiment and method of adjustment of this device of being exclusively used in.
Background technology
Synchrotron radiation X AFS spectrum experimental system has become a kind of effective means of the research structure of matter, serves multidisciplinary field, for example, and life science, field of new, Environmental Health field and industrial application etc.
The XAFS spectrum is utilized double-crystal monochromator to scan by photon energy and is measured.Monoenergetic light beam normal incidence from monochromator arrives sample, and for the photon absorption of sample variation of different-energy, the variation of the light intensity photon energy before and after the detection sample namely can obtain the XAFS spectrum.This XAFS spectrum is analyzed the structural information that namely can obtain in sample.
Along with going deep into of the energy, environment and new material the reach of science and related science research thereof, people need to know the architectural characteristic of film, device surface, solid-solid and the solid-liquid interface of various functions, yet conventional XAFS experimental system can't obtain the structural information of sample surfaces.So, glancing incidence XAFS(Grazing-incidence Absorption Fine Structure, GXAFS have appearred) and the spectrum experimental system.
When X ray incides material surface with minimum angle, its penetration depth sharply diminishes, when the grazing angle of X ray during less than the relevant special angle (for example critical angle) of a material, the X ray of incident is all reflected, only have an effect with material surface, only comprise like this structural information of material surface in the X ray of outgoing.This phenomenon is namely the physical basis of glancing incidence XAFS spectrum experiment.
some external laboratories, as the KEK(of Japan country high energy physics laboratory) and SPRING-8, ESRF(Europe synchrotron radiation mechanism of France) and U.S. APS(American Physical Society (APS)), the advanced light source synchrotron radiation of ALS(mechanism) and BNL(Brooker Hei Wen National Laboratory), the XAFS experimental technique of multiple film sample has been developed in domestic laboratory such as the NSRL in Hefei and Beijing Synchrotron Radiation laboratory etc. successively, obtained some solid surface, the structure of interface and film, surface catalysis and chemisorption have been obtained, the reconstruct of surface and interface atomic structure, the characteristics such as diffusion and stress relaxation.Yet, in experiment, how according to the characteristic of x-ray source and detector improve signal to noise ratio (S/N ratio), the interference that reduces parasitic light or diffraction peak remains has challenging problem.
Existing general scheme is to adopt θ-2 θ steering angle instrument, and its setting principle as shown in Figure 1.Fig. 1 schematically shows the schematic diagram that θ in prior art-2 θ steering angle instrument is used for glancing incidence XAFS experiment, X ray through monochromator incides on sample through front ionization chamber, sample stage is fixed on axle bed, and axle bed itself can rotate (θ rotation) around angle measurement platform central shaft.Detector (being generally the NaI scintillation detector) is fixed on armshaft, armshaft also can sway (2 θ rotate).Whole turntable is placed on an electric lifting platform, to adjust its vertical height.Fix a fluorescence ionization chamber to receive the fluorescence signal of sample on the rotary table base above sample stage.
There are the following problems for this set: the initial position of sample is difficult to accurate location.And in this set, the rotational angle of sample is difficult to accurate adjustment.In addition, the detection noise of this set is large, adopt the spectrum of low quality.
Summary of the invention
In order to overcome one or more in above-mentioned problems of the prior art, the embodiment of the present application provides a kind of device of glancing incidence XAFS experiment and method of adjustment of this device of being exclusively used in.
The embodiment of the present application provides a kind of device that is exclusively used in glancing incidence XAFS experiment, comprising:
Device for generation of the required X ray of described glancing incidence XAFS experiment;
Front slit is used for limiting the size of the X ray that described x-ray source sends;
The first lifting table is used for described front slit is installed, and makes the lifting on the direction vertical with the optical axis direction of described X ray of described front slit;
Specimen holder is used for the carrying sample, and the surface of described sample interacts with X ray from described front slit outgoing;
Universal stage is used for described specimen holder is installed, and makes the sample on described specimen holder rotate, to obtain required X ray glancing incidence angle;
The second lifting table is used for described universal stage is installed, and makes the lifting on the direction vertical with the optical axis direction of described X ray of described universal stage;
Rear slit is for the size of the full-reflection X ray after the surface interaction of restriction and described sample;
The 3rd lifting table is used for described rear slit is installed, and makes the lifting on the direction vertical with described X ray of described rear slit;
The pedestal lifting unit is used for described the first lifting table, described the second lifting table and described the 3rd lifting table are installed, and makes described the first lifting table, the second lifting table and the lifting on the direction vertical with the optical axis direction of described X ray of described the 3rd lifting table;
The first detector is used for surveying the fluorescence signal that sends from described sample;
The second detector is used for surveying the X ray signal from described rear slit outgoing.
On the basis of aforementioned structure, can also comprise the slit assembly, be arranged between described specimen holder and described the first detector; Described slit assembly comprises one group of uneven blade and has focus.And the center line of described sample to the distance of the table top of described universal stage is the focal length of described slit assembly.
On the basis of previous embodiment, can be provided with light shield on described the first detector.
The embodiment of the present application also provides a kind of method of adjustment of aforementioned means, comprising:
The adjusting base lifting unit makes described pedestal lifting unit reach the vertical height that is complementary with collimated light beam;
Open front slit, remove sample, regulate the height of described rear slit on the direction vertical with the optical axis of described X ray by the 3rd lifting table, until the output of the second detector reaches maximum;
Before regulating, the seam of slit is wide, and regulates the height of described front slit on the direction vertical with the optical axis of X ray by the first lifting table, until the output of the second detector reaches maximum;
Sample is placed on specimen holder, regulates the height of described specimen holder on the direction vertical with the optical axis of X ray by the second lifting table, until half when reaching maximum of the output of the second detector; Then drive universal stage, until the output of the second detector reaches maximum; Repeated vertical is regulated the step of described specimen holder, until half when reaching maximum of the output of described the second detector, and when clockwise and counterclockwise both direction rotated described universal stage, the output of described the second detector all reduced.
On the basis of above step, can also comprise: according to the required described universal stage of glancing incidence angle rotation; Described rear slit is set to the distance of described specimen holder, arrives the distance of described specimen holder according to described glancing incidence angle, described rear slit, calculate and arrange the upright position of described rear slit; Rotate described universal stage, until the output of described the second detector reaches maximal value.
The device that is exclusively used in glancing incidence XAFS experiment that the embodiment of the present application provides, replaced sample holder in conventional XAFS experimental system and the structure of probe portion, the formation of can being combined with the XAFS of routine experimental system has the hardware environment that realizes glancing incidence XAFS experiential function.
The device that is exclusively used in glancing incidence XAFS experiment that employing the embodiment of the present application provides and the method for adjustment of this device, before and after adjust after the wide and vertical height of the seam of slit, sample is placed on specimen holder, regulate specimen holder height in vertical direction by the second lifting table, then drive universal stage, until the output of the second detector reaches maximum; Repeated vertical is regulated the step of specimen holder, until half when reaching maximum of the output of the second detector, and when clockwise and counterclockwise both direction rotation universal stage, the output of the second detector all reduces.By such adjustment mode, sample can be adjusted to beam center and surperficial parallel with light beam, so just realized accurately setting fast of sample initial position, and can accurately adjust sample angle, and obtain the experimental detection data of sample with high s/n ratio, obtain high-quality glancing incidence XFAS experimental spectrum.
In this device, adopted two kinds of highly-sensitive detectors, can survey simultaneously fluorescence and full-reflection X light signal that sample produces.The X-ray signal that the X-ray signal intensity ratio normal incidence state sample that produces due to glancing incidence state sample produces is low, thereby highly sensitive detector can guarantee to adopt the spectrum quality.And the second detector supports sample position to set, so that form θ-2 θ detection mode between the second detector and sample.In addition, in this device, by on the detector mouth of fluorescent probe (i.e. the first detector), light shield being set, reduced the scattering back end that when propagating in air due to the X-ray signal, the generation scattering causes, reduced the detection noise, improved and adopted the spectrum quality.
In the XAFS spectrum was adopted the spectrum process, the silicon substrate of sample can produce diffraction peak, and the existence of diffraction peak can destroy the XAFS spectrum.Diffraction peak is exposed to X ray by the forward position silicon substrate of sample often and excites generation, the device that provides by using the embodiment of the present application, the generation of diffraction peak can be evaded in the upright position of micro-regulation sample, thereby has solved the problem of puzzlement Semiconductor Surface Structures by Slab test.
In addition, due to the rotation error of universal stage, position that might sample does not reach glancing incidence angle accurately after universal stage rotates.The method of adjustment that adopts the embodiment of the present application to provide, after required glancing incidence angle rotation universal stage, rear slit is set to the distance of specimen holder, according to glancing incidence angle, rear slit to the distance of specimen holder in conjunction with θ-2 θ relation, calculate and arrange the upright position of rear slit, then rotate universal stage, until the output of the second detector reaches maximal value.So just eliminate the universal stage rotation error, realized the accurate adjustment of the rotational angle of sample.
By referring to the accompanying drawing description of a preferred embodiment, above-mentioned and other objects, features and advantages of the present invention will be more obvious.
Description of drawings
Fig. 1 schematically shows the schematic diagram that θ in prior art-2 θ steering angle instrument is used for glancing incidence XAFS experiment;
Fig. 2 schematically shows the ultimate principle of glancing incidence XAFS spectrum experiment;
Fig. 3 schematically shows the side-looking structural representation of the device that is exclusively used in glancing incidence XAFS experiment of the embodiment of the present application;
Fig. 4 schematically shows a kind of universal stage in the embodiment of the present application and the relative position schematic diagram of sample;
Fig. 5 schematically shows the fluorescent X-ray detector schematic diagram with this slit assembly;
Fig. 6 schematically shows the process flow diagram of method of adjustment of the device that is exclusively used in glancing incidence XAFS experiment of the embodiment of the present application
Fig. 7 A and Fig. 7 B show the adjustment schematic diagram of sample initial position in the embodiment of the present application;
Fig. 8 schematically shows the mechanical construction drawing of the device that is exclusively used in glancing incidence XAFS experiment of the embodiment of the present application;
Fig. 9 schematically shows and uses the glancing incidence XAFS spectrum that device that the embodiment of the present application provides and method of adjustment obtain.
Embodiment
Before describing the device that is exclusively used in glancing incidence XAFS experiment of the embodiment of the present application, the ultimate principle of glancing incidence XAFS spectrum experiment is described first.
Fig. 2 schematically shows the ultimate principle of glancing incidence XAFS spectrum experiment.Make X ray 11 with the glancing incidence angle glancing incidence that is slightly less than critical angle to sample S, the X ray 11 of incident in the full emission of sample S surface generation, is only that several nanometers are to the material effect (factor analysis such as concrete penetration depth and the energy of X ray and material itself) of tens nanometers with sample S surface thickness.The fluorescence 13 that this surface produces comprises sample surfaces structure of matter information.Carry out Single energy X ray absorptionmetry scanning surveying the element absorption limit, receive fluorescence 13 by fluorescent probe FD simultaneously, namely can obtain the surperficial XAFS spectrum of the certain depth of sample.
Next the device that is exclusively used in glancing incidence XAFS experiment of the embodiment of the present application is described.
Fig. 3 schematically shows the side-looking structural representation of the device that is exclusively used in glancing incidence XAFS experiment of the embodiment of the present application, and this device comprises: for generation of device 201, front slit 202, the first lifting table 203, specimen holder 204, universal stage 205, the second lifting table 206, rear slit 207, the 3rd lifting table 208, the first detector 209 and second detector 210 of the required X ray of glancing incidence XAFS experiment.
Wherein, front slit 202, the first lifting table 203, specimen holder 204, universal stage 205, the second lifting table 206, rear slit 207, the 3rd lifting table 208, the first detector 209 and the second detector 210 can all be positioned on a pedestal lifting unit 211, this pedestal lifting unit 211 is used for the first lifting table 203, the second lifting table 206 and the 3rd lifting table 208 are installed, and makes the lifting simultaneously on the direction vertical with the optical axis direction of X ray of the first lifting table 203, the second lifting table 206 and the 3rd lifting table 208.The optical axis direction of X ray can be as shown in dotted line F in Fig. 3.
This pedestal lifting unit 211 can comprise installation base plate 211a and the 4th lifting table 211b, this installation base plate 211a is used for installing the first lifting table 203, the second lifting table 206 and the 3rd lifting table 208, the 4th lifting table 211b is used for installation base plate 211a is installed, and makes installation base plate 211a lifting on the direction vertical with the optical axis direction of X ray.The 4th lifting table 211b can be manual or electric lifting platform.Can adjust whole device height in vertical direction by pedestal lifting unit 211.
This pedestal lifting unit 211 can be fixed on slide block 212, makes whole device to slide on the direction that is parallel to the X ray optical axis.
In device shown in Figure 3, the device 201 of testing required X ray for generation of glancing incidence XAFS can have various structures.For example, this device 201 can comprise synchrotron radiation light source, double-crystal monochromator etc.The synchrotron radiation light source covering visible light is to the hard X ray of hundreds of keV, has that high strength, high collimation, emission angle are little, wide spectrum, has time structure, polarizability is arranged, certain coherence is arranged, the series of advantages such as can accurately calculate.According to bragg's formula, adopt double-crystal monochromator, can realize the adjustable X ray energy scan of the glancing incidence XAFS desired monoenergetic of experiment.Certainly, device 201 also can adopt other the structure that can produce required X ray.
Front slit 202 is used for being defined for the size of the X ray that the device 201 that produces the required X ray of glancing incidence XAFS experiment sends.The seam of front slit 202 is wide can pass through manual adjustments.
The first lifting table 203 is arranged on front slit 202 belows, is used for making the lifting in vertical direction of front slit 202.The first lifting table 203 can adopt the lifting table of Japanese fine horse river this model of KZG06030-C, the adjustment precision of this lifting table is 0.05 μ m, this lifting table can be driven by DS102 controller (a kind of controllor for step-by-step motor), can realize controlling manually or automatically.
Specimen holder 204 is used for carrying sample S.The X ray of slit 202 outgoing and the sample S on specimen holder 204 interact in the past, produce fluorescence and total reflection light.
Universal stage 205 is used for specimen holder 204 is installed, and makes specimen holder 204(namely make sample S) rotate, to obtain required X ray glancing incidence angle.The turning axle of universal stage 205 can be arranged in the intersection point place of the dotted line F of Fig. 3 and L and perpendicular to paper.Sample S surface also can be perpendicular to paper.When universal stage 205 rotated, sample S rotated, and the glancing incidence angle of X ray also changes.
One of design main points of specimen holder 204 are to make the rotating shaft of universal stage 205 along the surface of the surperficial bearing of trend process sample of sample S, can realize so the movement of vertical direction can not occuring when sample glancing incidence angle changes.Fig. 4 schematically shows a kind of universal stage in the embodiment of the present application and the relative position schematic diagram of sample, and in this figure, the rotating shaft of universal stage 205 (shown in dotted line) is along the surperficial bearing of trend of the sample S surface through sample.
Specimen holder 204 can be designed as dismountable structure, is convenient to like this installation of sample S.
The second lifting table 206 is used for 205 universal stages are installed, and makes universal stage 205 lifting on the direction vertical with the optical axis direction of X ray.This second lifting table 206 also can adopt the lifting table of Japanese fine horse river this model of KZG06030-C.Universal stage 205 can adopt the universal stage of Japanese fine horse river this model of KRW04360, and adjusting precision is 10 rads.These two all can be driven universal stage 205 and the second lifting table 206 by the DS102 controller, can realize controlling manually or automatically.
By universal stage 205 and the second lifting table 206, can carry out the VTOL (vertical take off and landing) of sample S and the setting of turned position.
Rear slit 207 is used for limiting the size of the full-reflection X ray after surface interaction with sample S.Rear slit 207 is slits of fixed width.Can select the wide slit of different seams as rear slit 207.
Slit 207 after the 3rd lifting table 208 is used for installing, and make the lifting on the direction vertical with X ray of rear slit 207.The 3rd lifting table 208 also can adopt the lifting table of Japanese fine horse river this model of KZG06030-C.The 3rd lifting table also can be driven by the DS102 controller, can realize manual or electronic control.
The first detector 209 is for the fluorescent probe of surveying the fluorescence signal that sends from sample S.For example, can adopt model is the fluorescent probe of LYTLE model.The probe face of this LYTLE fluorescent probe vertically downward, to receive the fluorescence signal that sends from sample S.Fluorescent probe 209 can be arranged on detector carriage 214, and detector carriage 214 can be arranged on the second lifting table 206, keeps fixed range between fluorescent probe 209 and specimen holder 204, and detector 209 and specimen holder 204 synchronization liftings.
Can be provided with slit assembly (not shown) between fluorescent probe 209 and specimen holder 204.This slit assembly can comprise one group of uneven blade, and has focus.The center line of sample S (as shown in the dot-and-dash line in Fig. 4) to the distance of slit assembly is the focal length of slit assembly.Particularly, this slit assembly can adopt the fluorescent X-ray detector (Fluorescent x-ray detector) that EXAFS company produces.Fig. 5 schematically shows the fluorescent X-ray detector schematic diagram with this slit assembly.In the application's embodiment, the slit assembly that the said firm provides is separated independent use from the fluorescent X-ray detector, realize purpose of the present invention.By using this slit assembly, all can be received by fluorescent probe 209 at the X ray of focus place all directions, thereby the X ray that fluorescent probe 209 receives is maximized.
In addition, 209 mouthfuls of fluorescent probes can arrange light shield, the scattering back end that when propagating in air due to the X-ray signal to reduce, the generation scattering causes.
The second detector 210 is used for surveying the X ray signal from rear slit 207 outgoing.This second detector 210 can be photodiode (PD), and this photodiode can be surveyed from the intensity of the X ray of rear slit 207 outgoing.The second detector 210 can be arranged on the 3rd lifting table 208 together with rear slit 207, and like this, the second detector 210 and rear slit 207 all have adjustment degree of freedom in vertical direction.
The 3rd lifting table 208 can be arranged on on linear slide platform 215, by this linear slide platform 215, can carry out the long distance of level and manually adjust.The glide direction of the 3rd lifting table 208 is parallel with the optical axis direction of X ray.Because rear slit 207 and the second detector 210 all are arranged on the 3rd lifting table 208, like this, rear slit 207 and the second detector 210 also can slide in the horizontal direction.That is to say, rear slit 207 and the second detector 210 not only have the adjusting degree of freedom on vertical direction, also have the adjusting degree of freedom on horizontal direction.By slit 207 and the second detector 210 after sliding in the horizontal direction, can fine adjustment after horizontal range between slit 207 and sample S.
In addition, in device shown in Figure 3, the first lifting table 203 and the second lifting table 206 all can be arranged on cushion block 213, are convenient to like this adjust the vertical height of first, second, and third lifting table.
The below describes the method for adjustment that is exclusively used in the device of glancing incidence XAFS experiment shown in Figure 3.Fig. 6 schematically shows the process flow diagram of method of adjustment of the device that is exclusively used in glancing incidence XAFS experiment of the embodiment of the present application.The method comprises the steps:
Step S31, adjusting base lifting unit make the pedestal lifting unit reach the vertical height that is complementary with collimated light beam.
Adjustment process is to carry out XAFS experiment preliminary work before, does not need device 201 to send X ray, can simulate x-ray source by the light direction collimated light source consistent with X ray so and regulate.Particularly, can expose to X-ray at 2 with the X-ray sensitized paper, determine the beam direction of collimated light source by the locus of 2 hot spots.This collimated light source can adopt collimation laser.
In step S31, what carry out is a kind of coarse adjustment, take collimated light beam as benchmark, whole device is elevated to suitable height.
Step S32, open front slit, remove sample, the height of slit on the direction vertical with the optical axis of X ray after regulating by the 3rd lifting table is until the output of the second detector reaches maximum.At this moment, show the beam center collimation of rear slit and collimated light source, that is to say, with the beam center collimation of X ray.
Before step S33, adjusting, the seam of slit is wide, and the height of slit on the direction vertical with the optical axis of X ray before regulating by the first lifting table, until the output of the second detector reaches maximum.At this moment, before and after showing, slit all collimates with the beam center of collimated light source, that is to say, collimates with the beam center of X ray.By such setting, the light-beam position between the slit of front and back and the sectional dimension of light beam all are defined.
Step S34, sample is placed on specimen holder, regulates the height of specimen holder on the direction vertical with the optical axis of X ray by the second lifting table, until half when reaching maximum of the output of the second detector; Then drive universal stage, until the output of the second detector reaches maximum; Repeated vertical is regulated the step of specimen holder, until half when reaching maximum of the output of the second detector, and when clockwise and counterclockwise both direction rotated universal stage, the output of the second detector all reduced.At this moment, show that the surface of sample is parallel with collimated light beam, and sample is positioned in the middle of light beam.
Particularly, as shown in Fig. 7 A and Fig. 7 B, Fig. 7 A and Fig. 7 B show the adjustment schematic diagram of sample initial position in the embodiment of the present application.For convenience of explanation, amplify for the size of collimated light beam in Fig. 7 A and Fig. 7 B.
If the surface of sample is not parallel with collimated light beam, and sample is not positioned in the middle of collimated light beam, as shown in Fig. 7 A, and when rotating universal stage when making sample be rotated counterclockwise, the collimated light beam cross section increase that sample blocks, the output of the second detector reduces.And when rotating universal stage when making sample turn clockwise, sample blocks collimated light beam cross section diminishes, thereby the output of the second detector increases.
If the surface of sample is parallel with collimated light beam, and sample is positioned at the centre of collimated light beam, as shown in Fig. 7 B, when the sample that rotates rotary table clockwise and when being rotated counterclockwise, sample blocks collimated light beam cross section all increases, and the output of the second detector all reduces.
Step S34 is the process of " small change " in fact, and by the adjustment of step S34, making sample be positioned at grazing angle is zero position.
Pass through above-mentioned step S31 after the step S34, namely completed accurately arranging fast of sample initial position.
The method of adjustment that the embodiment of the present application provides can also comprise following step:
Step S35, rotate universal stage according to required glancing incidence angle (for example, 0.15 degree).
Step S36, rear slit is set to the distance of specimen holder, to the distance of specimen holder and in conjunction with θ-2 θ relation, calculates and arrange the upright position of rear slit according to glancing incidence angle, rear slit.
According to the measuring principle of θ-2 θ, when incident ray rotated θ, the second detector need to change the angle of 2 θ.Specific to device as shown in Figure 3, rotate universal stage after the step S34 when obtaining the glancing incidence angle, the upright position of the second detector changes.
Step S36 calculates by theory the upright position that has calculated rear slit, and arranges.
Step S37, rotation universal stage are until the output of the second detector reaches maximal value.
Because there is rotation error in universal stage, thereby the glancing incidence angle after rotating through step S35 may be not accurate enough.Set up the upright position of rear slit by step S36 after, just obtain the accurate location of rear slit, made the light signal that incides on the second detector through rear slit maximum by rotating universal stage, just can realize the accurate adjustment of sample glancing incidence angle.
Can find out, above-mentioned steps S35-S37 is actually and has played the effect that the glancing incidence angle is checked, and then has guaranteed the accurate adjustment of glancing incidence angle.
By after move rear slit and the second detector this to combination, per sample to the distance of rear slit and the vertical range of rear its initial position of slot distances, can adjust the glancing incidence angle of sample.
The above method of adjustment that provides in the embodiment of the present invention can be compiled into by computer implemented program software, thereby can realize the robotization of whole method of adjustment.
Fig. 8 schematically shows the mechanical construction drawing of the device that is exclusively used in glancing incidence XAFS experiment of the embodiment of the present application, please notes the device that has omitted in this figure for generation of the required X ray of glancing incidence XAFS experiment.Whole device builds on lifting installing plate 501, and base platform is installed and regulated the height of single unit system by the hand-operated lifting platform.The hand-operated lifting platform is fixed on slide block, and slide block can move along optical axis direction on the experiment table track.This part by AH long-range translation stage 502, linear bearing assembly 510, socket head cap screw (GBT70.1-2000) 526 and 525 and lifting installation base plate 511 realize.
The Far Left of device is front slit 509, and the seam of this slit is wide can manual adjustments.Front slit 509 is fixed on vertical electric lifting table 503 by gusset 508 and cushion block 504, and front slit 509 can carry out the upright position adjustment.The model of electric lifting platform 503 is Japanese fine horse river KZG06030-C, and it adjusts precision is 0.05 μ m.Electric lifting platform 503 is driven by the DS102 controller, can realize controlling manually or automatically.
Be specimen holder 514 after front slit 509, specimen holder 514 is fixed on vertical electric lifting table 503 and electrical turntable 506, can realize the VTOL (vertical take off and landing) of sample and the locus setting of rotation.The model of electrical turntable 506 is Japanese fine horse river KRW04360, and it adjusts precision is 10 rads.Electrical turntable 506 and VTOL (vertical take off and landing) platform 503 are all to be driven by the DS102 controller, can realize controlling manually or automatically.Electrical turntable 506 can be arranged on turntable erecting bed 505.
Specimen holder 514 is arranged on specimen holder installing plate 515, and specimen holder 514 has sample panel 516.One of design main points of specimen holder 514 are to make the rotating shaft of electrical turntable 506 along the surface of the surperficial bearing of trend process sample of sample.Specimen holder 514 is detachable, is convenient to sample and installs.
Specimen holder 514 tops are equipped with XRF detector 513, and the model of this detector is LYTLE, the probe face of this detector vertically downward, the fluorescence signal that sends to receive sample.Keep fixed range between this detector 513 and specimen holder 514.Slit assembly (not shown) can also be set between detector 513 and specimen holder 514.On the detector mouth of this detector 513, light shield can be set, the scattering back end that scattering causes occurs when propagating in air due to the X-ray signal to reduce.Detector 513 can be arranged on detector carriage gusset 520.
Specimen holder 514 back are rear slits 518, and it is wide that rear slit 518 has fixing seam, and are fixing by gusset 517 and pressing plate 519, and the wide available installation of slit of different seams can be arranged.Be photodiode 522 after rear slit 518, this photodiode 522 is arranged on detector installing plate 507, is used for surveying the X ray intensity by rear slit 518.Rear slit 518 and photodiode 522 all are arranged on vertical electric lifting table 521, make rear slit 518 and photodiode 522 all have vertical adjustment degree of freedom.The model of vertical electric lifting table 521 is Japanese fine horse river KZG06030-C, and it adjusts precision is 0.05 μ m.This electric lifting platform 521 can be driven by the DS102 controller, can realize controlling manually or automatically.
Electric lifting platform 521 is installed on a cover linear slide platform, comprises slide plate 523 and rebound 524, can carry out the long distance of level by this linear slide platform and manually move.The combination that rear slit 518 and photodiode 522 form not only has the adjustment degree of freedom of vertical direction, and have an adjustment degree of freedom on optical axis direction, thereby can be after accurately setting on optical axis direction distance between slit 518 and photodiode 522 and sample.
Reference numeral 537 in Fig. 8 is packing ring, and 538 is hexagonal nut (GBT6170-2000M4), and 525-536 is socket head cap screw (GBT70.1-2000).
Adopt the application's the device and the control method thereof that are exclusively used in glancing incidence XAFS experiment, can obtain one of following effect at least.
The device that is exclusively used in glancing incidence XAFS experiment that the embodiment of the present application provides, replaced sample holder in conventional XAFS experimental system and the structure of probe portion, the formation of can being combined with the XAFS of routine experimental system has the hardware environment that realizes glancing incidence XAFS experiential function.
The XAFS spectrometry device that adopts the embodiment of the present application to provide utilizes universal stage and the second lifting table, and sample is adjusted to beam center and surperficial parallel with light beam, has so just realized accurately setting fast of sample initial position.
The device of the embodiment of the present application, sample stage plane can be set accurately and read for angle and the upright position of X ray, reading accuracy and adjust precision and can reach respectively 10 rads (0.003 degree) and 0.05 μ m.
In this device, adopted two kinds of highly-sensitive detectors, can survey simultaneously fluorescence and full-reflection X light signal that sample produces.The X-ray signal that the X-ray signal intensity ratio normal incidence state sample that produces due to glancing incidence state sample produces is low, thereby highly sensitive detector can guarantee to adopt the spectrum quality.And the support sample position of this second detector is set, so that form θ-2 θ detection mode between the second detector and sample.In addition, in this device, by on the detector mouth of fluorescent probe, light shield being set, reduced the scattering back end that when propagating in air due to the X-ray signal, the generation scattering causes, reduced the detection noise, improved and adopted the spectrum quality.
In the XAFS spectrum was adopted the spectrum process, the silicon substrate of sample can produce diffraction peak, and the existence of diffraction peak can destroy the XAFS spectrum.Diffraction peak is exposed to X ray by the forward position silicon substrate of sample often and excites generation, the device that provides by using the embodiment of the present application, the generation of diffraction peak can be evaded in the upright position of micro-regulation sample, thereby has solved the problem of puzzlement Semiconductor Surface Structures by Slab test.
Fig. 9 schematically shows and uses the glancing incidence XAFS spectrum that device that the embodiment of the present application provides and method of adjustment obtain, and this spectrum comprises the sample surfaces structural information.This sample is the silicon substrate platinum plating, has the film of 100 μ m, and the glancing incidence angle is 0.15 degree.In this figure, horizontal ordinate is the photon energy of the Single energy X ray absorptionmetry of incident, and ordinate is the absorption coefficient of sample.
Although described the present invention with reference to several exemplary embodiments, should be appreciated that term used is explanation and exemplary and nonrestrictive term.The spirit or the essence that do not break away from invention because the present invention can specifically implement in a variety of forms, so be to be understood that, above-described embodiment is not limited to any aforesaid details, and should be in the spirit and scope that the claim of enclosing limits explain widely, therefore fall into whole variations in claim or its equivalent scope and remodeling and all should be the claim of enclosing and contain.

Claims (9)

1. one kind is exclusively used in the device that glancing incidence XAFS tests, and comprising:
Device for generation of the required X ray of described glancing incidence XAFS experiment;
Front slit is used for limiting the size of the described X ray that sends for generation of the device of the required X ray of described glancing incidence XAFS experiment;
The first lifting table is used for described front slit is installed, and makes the lifting on the direction vertical with the optical axis direction of described X ray of described front slit;
Specimen holder is used for the carrying sample, and the surface of described sample interacts with X ray from described front slit outgoing;
Universal stage is used for described specimen holder is installed, and makes the sample on described specimen holder rotate, to obtain required X ray glancing incidence angle;
The second lifting table is used for described universal stage is installed, and makes the lifting on the direction vertical with the optical axis direction of described X ray of described universal stage;
Rear slit is for the size of the full-reflection X ray after the surface interaction of restriction and described sample;
The 3rd lifting table is used for described rear slit is installed, and makes the lifting on the direction vertical with described X ray of described rear slit;
The pedestal lifting unit is used for described the first lifting table, described the second lifting table and described the 3rd lifting table are installed, and makes described the first lifting table, the second lifting table and the lifting on the direction vertical with the optical axis direction of described X ray simultaneously of described the 3rd lifting table;
The first detector is used for surveying the fluorescence signal that sends from described sample;
The second detector is used for surveying the X ray signal from described rear slit outgoing.
2. device according to claim 1, wherein, the rotating shaft of described universal stage is along the surperficial bearing of trend of the described sample surface through described sample.
3. device according to claim 1, also comprise the slit assembly, is arranged between described specimen holder and described the first detector; Described slit assembly comprises one group of uneven blade and has focus.
4. device according to claim 3, wherein, the center line of described sample to the distance of the table top of described universal stage is the focal length of described slit assembly.
5. device according to claim 1, wherein, be provided with light shield on described the first detector.
6. device according to claim 1, wherein, described the second detector is arranged on described the 3rd lifting table;
Described the 3rd lifting table is arranged on the linear slide platform, and the glide direction of described the 3rd lifting table on described linear slide platform is parallel with the optical axis direction of described X ray.
7. the described device of arbitrary claim according to claim 1-6, described pedestal lifting unit comprises:
Installation base plate is used for installing described the first lifting table, described the second lifting table and described the 3rd lifting table;
The 4th lifting table is used for described installation base plate is installed, and makes the lifting on the direction vertical with the optical axis direction of described X ray of described installation base plate.
8. method of adjustment as the described device of arbitrary claim in claim 1-7 comprises:
The adjusting base lifting unit makes described pedestal lifting unit reach the vertical height that is complementary with collimated light beam;
Open front slit, remove sample, regulate the height of described rear slit on the direction vertical with the optical axis of X ray by the 3rd lifting table, until the output of the second detector reaches maximum;
Before regulating, the seam of slit is wide, and regulates the height of described front slit on the direction vertical with the optical axis of X ray by the first lifting table, until the output of the second detector reaches maximum;
Sample is placed on specimen holder, regulates the height of described specimen holder on the direction vertical with the optical axis of X ray by the second lifting table, until half when reaching maximum of the output of the second detector; Then drive universal stage, until the output of the second detector reaches maximum; Repeated vertical is regulated the step of described specimen holder, until half when reaching maximum of the output of described the second detector, and when clockwise and counterclockwise both direction rotated described universal stage, the output of described the second detector all reduced.
9. method according to claim 8 also comprises:
According to the required described universal stage of glancing incidence angle rotation;
Described rear slit is set to the distance of described specimen holder, arrives the distance of described specimen holder according to described glancing incidence angle, described rear slit, calculate and arrange the upright position of described rear slit;
Rotate described universal stage, until the output of described the second detector reaches maximal value.
CN201310081613.8A 2013-03-14 2013-03-14 Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device CN103175857B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310081613.8A CN103175857B (en) 2013-03-14 2013-03-14 Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310081613.8A CN103175857B (en) 2013-03-14 2013-03-14 Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device

Publications (2)

Publication Number Publication Date
CN103175857A true CN103175857A (en) 2013-06-26
CN103175857B CN103175857B (en) 2015-06-03

Family

ID=48635859

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310081613.8A CN103175857B (en) 2013-03-14 2013-03-14 Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device

Country Status (1)

Country Link
CN (1) CN103175857B (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104267055A (en) * 2014-10-10 2015-01-07 中国科学院高能物理研究所 Synchrotron radiation energy stabilizing device and method
CN104932538A (en) * 2015-07-03 2015-09-23 中国计量科学研究院 A ray machine rotation apparatus
CN106288796A (en) * 2016-07-26 2017-01-04 中国科学院上海应用物理研究所 A kind of glancing incidence XAFS high-temp in-situ stove
CN106568579A (en) * 2016-11-04 2017-04-19 北京控制工程研究所 X-ray grazing-incidence reflecting-mirror effective area calibration method
CN107064197A (en) * 2017-06-12 2017-08-18 沈阳科晶自动化设备有限公司 A kind of automatic high flux x-ray fluorescence analyzer
CN107110798A (en) * 2014-12-25 2017-08-29 株式会社理学 Grazing incidence fluorescence x-ray analysis equipment and method
CN109342477A (en) * 2018-11-05 2019-02-15 广州市怡文环境科技股份有限公司 A kind of adaptive sample stage feedback system and control method for TXRF analyzer
CN109490335A (en) * 2018-11-13 2019-03-19 中国科学院上海应用物理研究所 A kind of micro- focusing experiment porch of synchrotron radiation applications

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03160353A (en) * 1989-11-20 1991-07-10 Toshiba Corp Fluorescent x-ray analysis and fluorescent x-ray spectrometer
JPH05188019A (en) * 1991-07-23 1993-07-27 Hitachi Ltd X-ray composite analysis device
JPH07229862A (en) * 1994-02-16 1995-08-29 Nec Corp Total reflection fluorescence x-ray analyzer
WO2003048745A2 (en) * 2001-12-04 2003-06-12 X-Ray Optical Systems, Inc. X-ray fluorescence analyser for analysing fluid streams using a semiconductor-type detector and focusing means
JP2004333131A (en) * 2003-04-30 2004-11-25 Rigaku Corp Total reflection fluorescence xafs measuring apparatus
JP3613784B2 (en) * 1999-07-20 2005-01-26 株式会社ムサシノエンジニアリング In-situ total reflection fluorescent XAFS measuring device
CN2938083Y (en) * 2006-08-23 2007-08-22 北京普析通用仪器有限责任公司 Mechanical structure for regulating position of X-ray tube
CN101551345A (en) * 2009-05-20 2009-10-07 中国科学院长春光学精密机械与物理研究所 Spectrometer based on X ray inspired light source
CN102636508A (en) * 2012-03-20 2012-08-15 中国科学院上海应用物理研究所 Sample platform used for grazing incidence XAFS method

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03160353A (en) * 1989-11-20 1991-07-10 Toshiba Corp Fluorescent x-ray analysis and fluorescent x-ray spectrometer
JPH05188019A (en) * 1991-07-23 1993-07-27 Hitachi Ltd X-ray composite analysis device
JPH07229862A (en) * 1994-02-16 1995-08-29 Nec Corp Total reflection fluorescence x-ray analyzer
JP3613784B2 (en) * 1999-07-20 2005-01-26 株式会社ムサシノエンジニアリング In-situ total reflection fluorescent XAFS measuring device
WO2003048745A2 (en) * 2001-12-04 2003-06-12 X-Ray Optical Systems, Inc. X-ray fluorescence analyser for analysing fluid streams using a semiconductor-type detector and focusing means
JP2004333131A (en) * 2003-04-30 2004-11-25 Rigaku Corp Total reflection fluorescence xafs measuring apparatus
CN2938083Y (en) * 2006-08-23 2007-08-22 北京普析通用仪器有限责任公司 Mechanical structure for regulating position of X-ray tube
CN101551345A (en) * 2009-05-20 2009-10-07 中国科学院长春光学精密机械与物理研究所 Spectrometer based on X ray inspired light source
CN102636508A (en) * 2012-03-20 2012-08-15 中国科学院上海应用物理研究所 Sample platform used for grazing incidence XAFS method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
HIROYUKI OYANAGI: "A New Apparatus for Polarized X-ray Absorption Fine Structure Using Grazing-Incidence Fluorescence Excitation", 《JOURNAL OF SYNCHROTRON RADIATION》, vol. 5, 31 December 1998 (1998-12-31), pages 48 - 53 *
LIN XIAOYAN ET AL.: "Characterization and applications of a new tabletop confocal micro X-ray fluorescence setup", 《NUCLEAR INSTRUMENTS AND METHODS IN PHYSICS RESEARCH》, vol. 266, no. 11, 31 December 2008 (2008-12-31), pages 2638 - 2642, XP 029235451, DOI: doi:10.1016/j.nimb.2007.12.064 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104267055A (en) * 2014-10-10 2015-01-07 中国科学院高能物理研究所 Synchrotron radiation energy stabilizing device and method
US10302579B2 (en) 2014-12-25 2019-05-28 Rigaku Corporation Grazing incidence x-ray fluorescence spectrometer and grazing incidence x-ray fluorescence analyzing method
CN107110798B (en) * 2014-12-25 2019-08-16 株式会社理学 Grazing incidence fluorescence x-ray analysis equipment and method
CN107110798A (en) * 2014-12-25 2017-08-29 株式会社理学 Grazing incidence fluorescence x-ray analysis equipment and method
CN104932538A (en) * 2015-07-03 2015-09-23 中国计量科学研究院 A ray machine rotation apparatus
CN106288796A (en) * 2016-07-26 2017-01-04 中国科学院上海应用物理研究所 A kind of glancing incidence XAFS high-temp in-situ stove
CN106568579A (en) * 2016-11-04 2017-04-19 北京控制工程研究所 X-ray grazing-incidence reflecting-mirror effective area calibration method
CN107064197A (en) * 2017-06-12 2017-08-18 沈阳科晶自动化设备有限公司 A kind of automatic high flux x-ray fluorescence analyzer
CN109342477A (en) * 2018-11-05 2019-02-15 广州市怡文环境科技股份有限公司 A kind of adaptive sample stage feedback system and control method for TXRF analyzer
CN109490335A (en) * 2018-11-13 2019-03-19 中国科学院上海应用物理研究所 A kind of micro- focusing experiment porch of synchrotron radiation applications

Also Published As

Publication number Publication date
CN103175857B (en) 2015-06-03

Similar Documents

Publication Publication Date Title
Kirby et al. A low-background-intensity focusing small-angle X-ray scattering undulator beamline
Campbell et al. FIGARO: The new horizontal neutron reflectometer at the ILL
Lubeck et al. A novel instrument for quantitative nanoanalytics involving complementary X-ray methodologies
Wang et al. A dedicated powder diffraction beamline at the advanced photon source: commissioning and early operational results
US7929667B1 (en) High brightness X-ray metrology
Matsushita et al. A fast X-ray absorption spectrometer for use with synchrotron radiation
Schulz A direct method of determining preferred orientation of a flat reflection sample using a Geiger counter X‐ray spectrometer
Schlossman et al. A synchrotron x-ray liquid surface spectrometer
KR101275528B1 (en) High-resolution x-ray diffraction measurement with enhanced sensitivity
Kastengren et al. The 7BM beamline at the APS: a facility for time-resolved fluid dynamics measurements
EP2628030B1 (en) Remotely-aligned arcuate detector array for high energy x-ray imaging
US7920676B2 (en) CD-GISAXS system and method
Engström et al. A submicron synchrotron X-ray beam generated by capillary optics
CN1226590C (en) Apparatus for measuring film thickness formed on object, apparatus and method for measuring spectral reflectance of object, and apparatus and method of inspecting foreign material on object
US9606073B2 (en) X-ray scatterometry apparatus
Haubold et al. JUSIFA—A new user‐dedicated ASAXS beamline for materials science
Rehm et al. Kookaburra: the ultra-small-angle neutron scattering instrument at OPAL
Kavčič et al. Design and performance of a versatile curved-crystal spectrometer for high-resolution spectroscopy in the tender x-ray range
US7113566B1 (en) Enhancing resolution of X-ray measurements by sample motion
US6947520B2 (en) Beam centering and angle calibration for X-ray reflectometry
JP2004294136A (en) X-ray diffraction device
US7680243B2 (en) X-ray measurement of properties of nano-particles
US10634628B2 (en) X-ray fluorescence apparatus for contamination monitoring
Kleymenov et al. Five-element Johann-type X-ray emission spectrometer with a single-photon-counting pixel detector
JP2012255769A (en) Compound x-ray analysis apparatus

Legal Events

Date Code Title Description
PB01 Publication
C06 Publication
SE01 Entry into force of request for substantive examination
C10 Entry into substantive examination
GR01 Patent grant
C14 Grant of patent or utility model