CN103175857B - 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 PDFInfo
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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
Technical field
The present invention relates to modern structure of matter analytical approach-synchrotron radiation experimental technique, particularly relate to the method for adjustment that one is exclusively used in device that Grazing Incidence X-Ray Absorption Fine Structure (X-ray Absorption Fine Structure, XAFS) tests and this device.
Background technology
Synchrotron radiation X AFS composes a kind of effective means that experimental system has become the research structure of matter, serves multidisciplinary field, such as, and life science, field of new, Environmental Health field and industrial application etc.
XAFS spectrum utilizes double-crystal monochromator to be measured by photon energy scanning.From the monoenergetic light beam normal incidence of monochromator to sample, the photon absorption of sample for different-energy changes, and namely the change of the light intensity photon energy before and after detection sample can obtain XAFS spectrum.The structural information that namely can obtain in sample is analyzed to this XAFS spectrum.
That studies along with the energy, environment and new material the reach of science and related science thereof gos deep into, people need to know the architectural characteristic of the film of various function, device surface, solid-solid and solid-liquid interface, but conventional XAFS experimental system cannot obtain the structural information of sample surfaces.So, there is glancing incidence XAFS(Grazing-incidence Absorption Fine Structure, GXAFS) and compose experimental system.
When X ray incides material surface with minimum angle, its penetration depth sharply diminishes, when the grazing angle of X ray is less than relevant special angle (such as the critical angle) of a material, incident X ray is all reflected, only have an effect with material surface, in the X ray of such outgoing, only comprise the structural information of material surface.Namely this phenomenon is the physical basis that glancing incidence XAFS composes experiment.
Some external laboratories, KEK(country high energy physics laboratory as Japan) and SPRING-8, the ESRF(European synchronous radiation mechanism of France) and APS(American Physical Society (APS) of the U.S.), ALS(advanced light source synchronous radiation 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, obtain some solid surface, the structure of interface and film, obtain surface catalysis and chemisorption, surface and interface atomic structure reconstructs, the characteristics such as diffusion and stress relaxation.But in an experiment, the characteristic how according to x-ray source and detector improves signal to noise ratio (S/N ratio), reduce the interference of parasitic light or diffraction peak remains and have challenging problem.
Existing general scheme adopts θ-2 θ steering angle instrument, and its setting principle as shown in Figure 1.Fig. 1 schematically shows the schematic diagram that in prior art, θ-2 θ steering angle instrument is tested for glancing incidence XAFS, X ray through monochromator incides on sample through front ionization chamber, sample stage is fixed on axle bed, and axle bed itself can around angle measurement platform central axis (θ rotation).Detector (being generally NaI scintillation detector) is then fixed on armshaft, and armshaft also can sway (2 θ rotate).Whole turntable is placed on an electric lifting platform, to adjust its vertical height.Rotary table base above sample stage is fixed a fluorescence ionization chamber to receive the fluorescence signal of sample.
There are the following problems for this set: the initial position of sample is difficult to accurate location.And the rotational angle of sample is difficult to accurate adjustment in this set.In addition, the detection noise of this set is large, and it is of low quality to adopt spectrum.
Summary of the invention
One or more in order to what overcome in above-mentioned problems of the prior art, the embodiment of the present application provides a kind of method of adjustment being exclusively used in device that glancing incidence XAFS tests and this device.
The embodiment of the present application provides a kind of device being exclusively used in glancing incidence XAFS and testing, and comprising:
The device of the X ray needed for testing for generation of described glancing incidence XAFS;
Front slit, for limiting the size of the X ray that described x-ray source sends;
First lifting table, for installing described front slit, and makes described front slit be elevated on the direction vertical with the optical axis direction of described X ray;
Specimen holder, for carrying sample, the surface of described sample with interact from the X ray of described front slit outgoing;
Universal stage, for installing described specimen holder, and makes the sample on described specimen holder rotate, to obtain required X ray glancing incidence angles;
Second lifting table, for installing described universal stage, and makes described universal stage be elevated on the direction vertical with the optical axis direction of described X ray;
Rear slit, for limit with the surface interaction of described sample after the size of full-reflection X ray;
3rd lifting table, for installing described rear slit, and makes described rear slit be elevated on the direction vertical with described X ray;
Pedestal lifting unit, for installing described first lifting table, described second lifting table and described 3rd lifting table, makes described first lifting table, the second lifting table be elevated on the direction vertical with the optical axis direction of described X ray with described 3rd lifting table;
First detector, for detecting the fluorescence signal sent from described sample;
Second detector, for detecting the X ray signal from described rear slit outgoing.
On the basis of aforementioned structure, slit assembly can also be comprised, be arranged between described specimen holder and described 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 table top of described universal stage is the focal length of described slit assembly.
On the basis of previous embodiment, described first detector can be provided with light shield.
The embodiment of the present application additionally provides a kind of method of adjustment of aforementioned means, comprising:
Adjusting base lifting unit, makes described pedestal lifting unit reach the vertical height matched 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, until the output of the second detector reaches maximum by the 3rd lifting table;
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, until the output of the second detector reaches maximum by the first lifting table;
Sample is placed on specimen holder, regulates the height of described specimen holder on the direction vertical with the optical axis of X ray, until the half when output of the second detector reaches maximum by the second lifting table; Then universal stage is driven, until the output of the second detector reaches maximum; Repeated vertical regulates the step of described specimen holder, until the half when output of described second detector reaches maximum, and when clockwise and counterclockwise both direction rotates described universal stage, the output of described second detector all reduces.
On the basis of above step, can also comprise: rotate described universal stage according to required glancing incidence angles; The distance of described rear slit to described specimen holder is set, according to described glancing incidence angles, described rear slit to the distance of described specimen holder, calculates and the upright position of described rear slit is set; Rotate described universal stage, until the output of described second detector reaches maximal value.
What the embodiment of the present application provided be exclusively used in device that glancing incidence XAFS tests, instead of the structure of sample holder in conventional XAFS experimental system and probe portion, can be bonded with the XAFS experimental system of routine the hardware environment having and realize glancing incidence XAFS experiential function.
What adopt the embodiment of the present application to provide is exclusively used in the device of glancing incidence XAFS experiment and the method for adjustment of this device, after the wide and vertical height of the seam adjusting front and back slit, sample is placed on specimen holder, specimen holder height is in vertical direction regulated by the second lifting table, then universal stage is driven, until the output of the second detector reaches maximum; Repeated vertical regulates the step of specimen holder, until the half when output of the second detector reaches maximum, and when clockwise and counterclockwise both direction rotates universal stage, the output of the second detector all reduces.By such adjustment mode, sample can be adjusted to beam center and surface parallel with light beam, so just achieve the accurately setting fast of sample initial position, and accurately can adjust sample angle, and the experimental detection data of sample are obtained with high s/n ratio, obtain high-quality glancing incidence XFAS experimental spectrum.
In the apparatus, have employed two kinds of highly-sensitive detectors, fluorescence and the full-reflection X light signal of sample generation can be detected simultaneously.The X-ray signal produced due to the X-ray signal intensity ratio normal incidence state sample of glancing incidence state sample generation is low, and thus highly sensitive detector can ensure to adopt spectrum quality.And sample position setting supported by the second detector, to make to form θ-2 θ detection mode between the second detector and sample.In addition, in the apparatus, by arranging light shield on the detector mouth of fluorescent probe (i.e. the first detector), decreasing the scattering back end caused owing to there is scattering when X-ray signal is propagated in atmosphere, reducing detection noise, improve and adopt spectrum quality.
Adopt in spectrum process in XAFS spectrum, the silicon substrate of sample can produce diffraction peak, and the existence of diffraction peak can destroy XAFS spectrum.Diffraction peak is exposed to X ray by the forward position silicon substrate of sample often and excites generation, by the device that application the embodiment of the present application provides, the upright position of micro-regulation sample, can evade the generation of diffraction peak, thus solves the problem of puzzlement Semiconductor Surface Structures by Slab test.
In addition, due to the rotation error of universal stage, likely the position of sample does not reach glancing incidence angles accurately after universal stage rotates.Adopt the method for adjustment that the embodiment of the present application provides, after rotating universal stage according to required glancing incidence angles, the distance of rear slit to specimen holder is set, according to glancing incidence angles, rear slit to the distance of specimen holder in conjunction with θ-2 θ relation, calculate and the upright position of rear slit is set, then universal stage is rotated, until the output of the second detector reaches maximal value.Thus eliminating the need universal stage rotation error, achieve the accurate adjustment of the rotational angle of sample.
By referring to accompanying drawing description of a preferred embodiment, above-mentioned and other objects, features and advantages of the present invention will be more obvious.
Accompanying drawing explanation
Fig. 1 schematically shows the schematic diagram that in prior art, θ-2 θ steering angle instrument is tested for glancing incidence XAFS;
Fig. 2 schematically shows the ultimate principle that glancing incidence XAFS composes experiment;
Fig. 3 schematically shows the side-looking structural representation being exclusively used in the device that glancing incidence XAFS tests of the embodiment of the present application;
Fig. 4 schematically shows the relative position schematic diagram of a kind of universal stage in the embodiment of the present application and sample;
Fig. 5 schematically shows the fluorescent X-ray detector schematic diagram with this slit assembly;
Fig. 6 schematically shows the process flow diagram being exclusively used in the method for adjustment of the device that glancing incidence XAFS tests of the embodiment of the present application
Fig. 7 A and Fig. 7 B shows the adjustment schematic diagram of sample initial position in the embodiment of the present application;
Fig. 8 schematically shows the mechanical construction drawing being exclusively used in the device that glancing incidence XAFS tests of the embodiment of the present application;
Fig. 9 schematically shows the glancing incidence XAFS that the application device that provides of the embodiment of the present application and method of adjustment obtain and composes.
Embodiment
Describe the embodiment of the present application be exclusively used in glancing incidence XAFS test device before, first describe glancing incidence XAFS compose experiment ultimate principle.
Fig. 2 schematically shows the ultimate principle that glancing incidence XAFS composes experiment.Make X ray 11 to be slightly less than the glancing incidence angles glancing incidence of critical angle to sample S, there is full transmitting on sample S surface in incident X ray 11, is only the material effect (concrete penetration depth with the factor such as the energy of X ray and material itself relevant) of a few nanometer to tens nanometers to 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 on detection element absorption limit, receive fluorescence 13 by fluorescent probe FD simultaneously, namely can obtain the surperficial XAFS spectrum of the certain depth of sample.
The device being exclusively used in glancing incidence XAFS experiment of following description the embodiment of the present application.
Fig. 3 schematically shows the side-looking structural representation being exclusively used in the device that glancing incidence XAFS tests of the embodiment of the present application, and this device comprises: device 201, front slit 202, first lifting table 203, specimen holder 204, universal stage 205, second lifting table 206, rear slit 207, the 3rd lifting table 208, first detector 209 and second detector 210 of the X ray needed for testing for generation of glancing incidence XAFS.
Wherein, front slit 202, first lifting table 203, specimen holder 204, universal stage 205, second lifting table 206, rear slit 207, the 3rd lifting table 208, first detector 209 and the second detector 210 all can be positioned on a pedestal lifting unit 211, this pedestal lifting unit 211, for installing the first lifting table 203, second lifting table 206 and the 3rd lifting table 208, makes the first lifting table 203, second lifting table 206 be elevated on the direction vertical with the optical axis direction of X ray with the 3rd lifting table 208 simultaneously.The optical axis direction of X ray can 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 for installing the first lifting table 203, second lifting table 206 and the 3rd lifting table 208,4th lifting table 211b, for installing installation base plate 211a, makes installation base plate 211a be elevated on the direction vertical with the optical axis direction of X ray.4th lifting table 211b can be manual or electric lifting platform.Whole device height in vertical direction can be adjusted by pedestal lifting unit 211.
This pedestal lifting unit 211 can be fixed on slide block 212, makes whole device being parallel to the square upward sliding of X ray optical axis.
In the device shown in Fig. 3, the device 201 of the X ray needed for testing for generation of glancing incidence XAFS can have various structure.Such as, this device 201 can comprise synchrotron radiation light source, double-crystal monochromator etc.Synchrotron radiation light source covering visible light, to the hard X ray of hundreds of keV, has that high strength, high collimation, emission angle are little, wide spectrum, has time structure, has polarizability, has certain coherence, the series of advantages such as accurately can to calculate.According to bragg's formula, adopt double-crystal monochromator, the adjustable X-ray energy scanning of monoenergetic required by glancing incidence XAFS experiment can be realized.Certainly, device 201 also can adopt other the structure that can produce required X ray.
The size of the X ray that front slit 202 sends for the device 201 being defined for the X ray produced needed for glancing incidence XAFS experiment.The seam of front slit 202 is wide can manually be regulated.
First lifting table 203 is arranged on below front slit 202, is provided for front slit 202 and is elevated in vertical direction.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 μm, 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 for carrying sample S.The in the past X ray of slit 202 outgoing and the sample S-phase interaction on specimen holder 204, generation fluorescence and total reflection light.
Universal stage 205 for installing specimen holder 204, and makes specimen holder 204(namely make sample S) rotate, to obtain required X ray glancing incidence angles.The turning axle of universal stage 205 can be arranged in dotted line F and L of Fig. 3 point of intersection and perpendicular to paper.Sample S surface also can perpendicular to paper.When universal stage 205 rotates, sample S rotates, and the glancing incidence angles of X ray also changes.
One of designing points of specimen holder 204 makes the rotating shaft of universal stage 205 along the surperficial bearing of trend of sample S through the surface of sample, can realize the movement that vertical direction can not occur when sample glancing incidence angles changes like this.Fig. 4 schematically shows the relative position schematic diagram of a kind of universal stage in the embodiment of the present application and sample, in this figure, the rotating shaft (shown in dotted line) of universal stage 205 along the surperficial bearing of trend of sample S through the surface of sample.
Specimen holder 204 can be designed as dismountable structure, is convenient to the installation of sample S like this.
Second lifting table 206 for installing 205 universal stages, and makes universal stage 205 be elevated 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 Adjustment precision is 10 rads.Both universal stage 205 and the second lifting table 206 all can be driven by DS102 controller, can realize controlling manually or automatically.
By universal stage 205 and the second lifting table 206, the VTOL (vertical take off and landing) of sample S and the setting of turned position can be carried out.
Rear slit 207 for limit with the surface interaction of sample S after the size of full-reflection X ray.Rear slit 207 is slits of fixed width.The slit that different seam can be selected wide is as rear slit 207.
3rd lifting table 208 for installing rear slit 207, and makes rear slit 207 be elevated on the direction vertical with X ray.3rd lifting table 208 also can adopt the lifting table of Japanese fine horse river this model of KZG06030-C.3rd lifting table also can be driven by DS102 controller, can realize manually or Electronic control.
First detector 209 is the fluorescent probes for detecting the fluorescence signal sent from sample S.Such as, model can be adopted to be the fluorescent probe of LYTLE model.The probe face of this LYTLE fluorescent probe vertically downward, to receive the fluorescence signal sent from sample S.Fluorescent probe 209 can be arranged in 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 lifting.
Slit assembly (not shown) can be provided with between fluorescent probe 209 and specimen holder 204.This slit assembly can comprise one group of uneven blade, and has focus.The center line (as illustrated by the dash-and-dot line in figure 4) of sample S to the distance of slit assembly is the focal length of slit assembly.Specifically, this slit assembly fluorescent X-ray detector (Fluorescent x-ray detector) that EXAFS company can be adopted to produce.Fig. 5 schematically shows the fluorescent X-ray detector schematic diagram with this slit assembly.In the embodiment of the application, slit assembly the said firm provided is separated and is used alone from fluorescent X-ray detector, realizes object 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, thus the X ray received by fluorescent probe 209 maximizes.
In addition, fluorescent probe 209 mouthfuls can arrange light shield, to reduce the scattering back end caused owing to there is scattering when X-ray signal is propagated in atmosphere.
Second detector 210 is for detecting the X ray signal from the outgoing of rear slit 207.This second detector 210 can be photodiode (PD), and this photodiode can detect the intensity of the X ray from the outgoing of rear slit 207.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.
3rd lifting table 208 can be arranged on on linear slide platform 215, by this linear slide platform 215, can carry out the manually adjustment of the long distance of level.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 are all be 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, rear slit 207 and the second detector 210 not only have the adjustment degree of freedom in vertical direction, also have the adjustment degree of freedom in horizontal direction.By slit 207 and the second detector 210 after sliding in the horizontal direction, can horizontal range after fine adjustment between slit 207 and sample S.
In addition, in the device shown in Fig. 3, the first lifting table 203 and the second lifting table 206 all can be arranged on cushion block 213, are convenient to the vertical height of adjustment first, second, and third lifting table like this.
The method of adjustment being exclusively used in the device that glancing incidence XAFS tests shown in Fig. 3 is described below.Fig. 6 schematically shows the process flow diagram being exclusively used in the method for adjustment of the device that glancing incidence XAFS tests of the embodiment of the present application.The method comprises the steps:
Step S31, adjusting base lifting unit, make pedestal lifting unit reach the vertical height matched with collimated light beam.
Adjustment process carries out the preliminary work before XAFS experiment, do not need device 201 to send X ray, so can be simulated x-ray source by the collimated light source that light direction is consistent with X ray and regulate.Specifically, can expose X-ray at 2 with X-ray sensitized paper, be determined 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 being regulated by the 3rd lifting table, until the output of the second detector reaches maximum.At this moment, show that the beam center of rear slit and collimated light source collimates, that is, collimate with the beam center of X ray.
Before step S33, adjustment, the seam of slit is wide, and the height of slit on the direction vertical with the optical axis of X ray before being regulated by the first lifting table, until the output of the second detector reaches maximum.At this moment, show that front and back slit all collimates with the beam center of collimated light source, that is, collimate 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 are all 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, until the half when output of the second detector reaches maximum by the second lifting table; Then universal stage is driven, until the output of the second detector reaches maximum; Repeated vertical regulates the step of specimen holder, until the half when output of the second detector reaches maximum, and when clockwise and counterclockwise both direction rotates universal stage, the output of the second detector all reduces.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.
Specifically, as shown in figures 7 a and 7b, Fig. 7 A and Fig. 7 B shows the adjustment schematic diagram of sample initial position in the embodiment of the present application.For convenience of explanation, in Fig. 7 A and Fig. 7 B, the size of collimated light beam is amplified.
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 Figure 7 A, then, when rotating universal stage and making sample be rotated counterclockwise, the collimated light beam cross section that sample blocks increases, and the output of the second detector reduces.And when rotating universal stage and making sample turn clockwise, the collimated light beam cross section that sample blocks diminishes, thus 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 Figure 7 B, then when rotating the sample of rotary table clockwise with when being rotated counterclockwise, the collimated light beam cross section that sample blocks all increases, and the output of the second detector all reduces.
Step S34 is the process of " small change " in fact, by the adjustment of step S34, and sample is positioned at position that grazing angle is zero.
After have passed through above-mentioned step S31 to step S34, namely complete 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, according to required glancing incidence angles (such as, 0.15 degree) rotate universal stage.
Step S36, the distance of rear slit to specimen holder is set, according to glancing incidence angles, rear slit to specimen holder distance and in conjunction with θ-2 θ relation, calculate and the upright position of rear slit be set.
According to the measuring principle of θ-2 θ, when incident ray rotates θ, the second detector needs the angle of change 2 θ.Specific to device as shown in Figure 3, after step S34, rotate universal stage when obtaining glancing incidence angles, the upright position of the second detector changes.
Step S36 has calculated the upright position of rear slit by theory calculate, and arranges.
Step S37, rotation universal stage, until the output of the second detector reaches maximal value.
Because universal stage exists rotation error, the glancing incidence angles thus after step S35 rotates 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, making 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 angles.
Can find out, above-mentioned steps S35-S37 is actually the effect serving and check glancing incidence angles, and then ensure that the accurate adjustment of glancing incidence angles.
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, the glancing incidence angles of sample can be adjusted.
The above method of adjustment provided in the embodiment of the present invention, can be compiled into by computer implemented program software, thus can realize the robotization of whole method of adjustment.
Fig. 8 schematically shows the mechanical construction drawing being exclusively used in the device that glancing incidence XAFS tests of the embodiment of the present application, please notes in this figure the device eliminated for generation of the X ray needed for glancing incidence XAFS experiment.Whole device builds on liftable mounting plate 501, and base platform is installed by hand-operated lifting platform and regulated the height of single unit system.Hand-operated lifting platform is fixed on slide block, and slide block can move along optical axis direction on experiment table track.This part is realized by AH long-range translational platform 502, linear bearing assembly 510, socket head cap screw (GBT70.1-2000) 526 and 525 and lifting installation base plate 511.
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, then before, slit 509 can carry out upright position adjustment.The model of electric lifting platform 503 is Japanese fine horse river KZG06030-C, and its Adjustment precision is 0.05 μm.Electric lifting platform 503 is driven by 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 its Adjustment precision is 10 rads.Electrical turntable 506 and VTOL (vertical take off and landing) platform 503 are all driven by 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 designing points of specimen holder 514 makes the rotating shaft of electrical turntable 506 along the surperficial bearing of trend of sample through the surface of sample.Specimen holder 514 is detachable, is convenient to sample and installs.
Be provided with XRF detector 513 above specimen holder 514, the model of this detector is LYTLE, the probe face of this detector vertically downward, to receive the fluorescence signal that sample sends.Fixed range is kept between this detector 513 and specimen holder 514.Slit assembly (not shown) can also be set between detector 513 and specimen holder 514.The detector mouth of this detector 513 can arrange light shield, to reduce the scattering back end caused owing to there is scattering when X-ray signal is propagated in atmosphere.Detector 513 can be arranged on detector carriage gusset 520.
Specimen holder 514 back is rear slit 518, and it is wide that rear slit 518 has fixing seam, fixed by gusset 517 and pressing plate 519, can have the available installation of slit that different seam is wide.Be photodiode 522 after rear slit 518, this photodiode 522 is arranged on detector installing plate 507, for detecting the X-ray intensity by rear slit 518.Rear slit 518 and photodiode 522 are all arranged on vertical electric lifting table 521, rear slit 518 and photodiode 522 are all had and vertically adjusts degree of freedom.The model of vertical electric lifting table 521 is Japanese fine horse river KZG06030-C, and its Adjustment precision is 0.05 μm.This electric lifting platform 521 can be driven by DS102 controller, can realize controlling manually or automatically.
Electric lifting platform 521 is installed on a set of linear slide platform, comprises slide plate 523 and rebound 524, can carry out the long distance of level manually move by this linear slide platform.The combination that rear slit 518 and photodiode 522 are formed not only has the adjustment degree of freedom of vertical direction, and the adjustment degree of freedom had on optical axis direction, thus can accurately set rear slit 518 and the distance between photodiode 522 and sample in the direction of the optical axis.
Reference numeral 537 in Fig. 8 is packing ring, and 538 be hexagonal nut (GBT6170-2000M4), 525-536 is socket head cap screw (GBT70.1-2000).
Adopt the device being exclusively used in glancing incidence XAFS experiment and the control method thereof of the application, at least can obtain one of following effect.
What the embodiment of the present application provided be exclusively used in device that glancing incidence XAFS tests, instead of the structure of sample holder in conventional XAFS experimental system and probe portion, can be bonded with the XAFS experimental system of routine the hardware environment having and realize glancing incidence XAFS experiential function.
The XAFS spectrometry device that theres is provided of the embodiment of the present application is provided, utilizes universal stage and the second lifting table, sample is adjusted to beam center and surface is parallel with light beam, so just achieve accurately setting fast of sample initial position.
The device of the embodiment of the present application, sample stage plane can set for the angle of X ray and upright position accurately and read, and reading accuracy and Adjustment precision can reach 10 rads (0.003 degree) and 0.05 μm respectively.
In the apparatus, have employed two kinds of highly-sensitive detectors, fluorescence and the full-reflection X light signal of sample generation can be detected simultaneously.The X-ray signal produced due to the X-ray signal intensity ratio normal incidence state sample of glancing incidence state sample generation is low, and thus highly sensitive detector can ensure to adopt spectrum quality.And the support sample position setting of this second detector, to make to form θ-2 θ detection mode between the second detector and sample.In addition, in the apparatus, by arranging light shield on the detector mouth of fluorescent probe, decreasing the scattering back end caused owing to there is scattering when X-ray signal is propagated in atmosphere, reducing detection noise, improve and adopt spectrum quality.
Adopt in spectrum process in XAFS spectrum, the silicon substrate of sample can produce diffraction peak, and the existence of diffraction peak can destroy XAFS spectrum.Diffraction peak is exposed to X ray by the forward position silicon substrate of sample often and excites generation, by the device that application the embodiment of the present application provides, the upright position of micro-regulation sample, can evade the generation of diffraction peak, thus solves the problem of puzzlement Semiconductor Surface Structures by Slab test.
Fig. 9 schematically shows the glancing incidence XAFS that the application device that provides of the embodiment of the present application and method of adjustment obtain and composes, and this spectrum comprises sample surfaces structural information.This sample is silicon substrate platinum plating, has the film of 100 μm, and glancing incidence angles is 0.15 degree.In this figure, horizontal ordinate is the photon energy of incident Single energy X ray absorptionmetry, and ordinate is the absorption coefficient of sample.
Although exemplary embodiment describe the present invention with reference to several, should be appreciated that term used illustrates and exemplary and nonrestrictive term.Spirit or the essence of invention is not departed from 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 explain widely in the spirit and scope that should limit in claim of enclosing, therefore fall into whole change in claim or its equivalent scope and remodeling and all should be claim of enclosing and contained.
Claims (7)
1. be exclusively used in the device that glancing incidence XAFS tests, comprise:
The device of the X ray needed for testing for generation of described glancing incidence XAFS;
Front slit, for limit described to test for generation of described glancing incidence XAFS needed for the size of X ray that sends of the device of X ray;
First lifting table, for installing described front slit, and makes described front slit be elevated on the direction vertical with the optical axis direction of described X ray;
Specimen holder, for carrying sample, the surface of described sample with interact from the X ray of described front slit outgoing;
Universal stage, for installing described specimen holder, and makes the sample on described specimen holder rotate, to obtain required X ray glancing incidence angles;
Second lifting table, for installing described universal stage, and makes described universal stage be elevated on the direction vertical with the optical axis direction of described X ray;
Rear slit, for limit with the surface interaction of described sample after the size of full-reflection X ray;
3rd lifting table, for installing described rear slit, and makes described rear slit be elevated on the direction vertical with described X ray;
Pedestal lifting unit, for installing described first lifting table, described second lifting table and described 3rd lifting table, makes described first lifting table, the second lifting table be elevated on the direction vertical with the optical axis direction of described X ray with described 3rd lifting table simultaneously;
First detector, for detecting the fluorescence signal sent from described sample;
Second detector, for detecting the X ray signal from described rear slit outgoing;
Wherein, the rotating shaft of described universal stage along the surperficial bearing of trend of described sample through the surface of described sample;
Described first detector is provided with light shield.
2. device according to claim 1, also comprises slit assembly, is arranged between described specimen holder and described first detector; Described slit assembly comprises one group of uneven blade and has focus.
3. device according to claim 2, 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.
4. device according to claim 1, wherein, described second detector is arranged on described 3rd lifting table;
Described 3rd lifting table is arranged on linear slide platform, and the glide direction of described 3rd lifting table on described linear slide platform is parallel with the optical axis direction of described X ray.
5. the device according to claim arbitrary in claim 1-4, described pedestal lifting unit comprises:
Installation base plate, for installing described first lifting table, described second lifting table and described 3rd lifting table;
4th lifting table, for installing described installation base plate, makes described installation base plate be elevated on the direction vertical with the optical axis direction of described X ray.
6. a method of adjustment for the device as described in claim arbitrary in claim 1-5, comprising:
Adjusting base lifting unit, makes described pedestal lifting unit reach the vertical height matched 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, until the output of the second detector reaches maximum by the 3rd lifting table;
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, until the output of the second detector reaches maximum by the first lifting table;
Sample is placed on specimen holder, regulates the height of described specimen holder on the direction vertical with the optical axis of X ray, until the half when output of the second detector reaches maximum by the second lifting table; Then universal stage is driven, until the output of the second detector reaches maximum; Repeated vertical regulates the step of described specimen holder, until the half when output of described second detector reaches maximum, and when clockwise and counterclockwise both direction rotates described universal stage, the output of described second detector all reduces.
7. method according to claim 6, also comprises:
Described universal stage is rotated according to required glancing incidence angles;
The distance of described rear slit to described specimen holder is set, according to described glancing incidence angles, described rear slit to the distance of described specimen holder, calculates and the upright position of described rear slit is set;
Rotate described universal stage, until the output of described second detector reaches maximal value.
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