CN1504744A - Method and apparatus for measuring and analyzing structure and component of combined sample - Google Patents
Method and apparatus for measuring and analyzing structure and component of combined sample Download PDFInfo
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- CN1504744A CN1504744A CNA021484392A CN02148439A CN1504744A CN 1504744 A CN1504744 A CN 1504744A CN A021484392 A CNA021484392 A CN A021484392A CN 02148439 A CN02148439 A CN 02148439A CN 1504744 A CN1504744 A CN 1504744A
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Abstract
The invention relates to a process and apparatus for measuring and analyzing the structure and component of a combination sample, wherein an X-ray source and an X-ray lens form incident light path, an energy detector is arranged on the diffraction light path, the divergent white light set out by the X-ray source is focused into parallel micro convergent beams onto the sample platform through an X-ray lens, then an energy detector receives the diffracted X-rays and fluorescent X-rays from the tested sample, and transmit them into the computer for data processing, thus obtaining the diffraction spectrum and fluorescence spectrum and analyzing the structure and constitution.
Description
Technical field:
The present invention relates to utilize simultaneously X-ray diffraction, XRF technology structure and composition to be carried out the method and the device of Measurement and analysis.
Background technology:
At present, when the crystal structure of material and composition are analyzed, adopt the X-ray diffraction technology usually.The most conventional is angular dispersion X-ray diffraction (being called for short XRD), adopt single wavelength X ray (monochromatic light, monochromatization behind monochromatization or the diffraction before the diffraction) irradiation material sample makes and does the scanning of θ-2 θ interlock between sample face and the detector, is met diffraction formula 2dsin θ=λ
0Diffracting spectrum (d is interplanar distance, is the structural parameters of specimen material that θ is an angle of diffraction, λ
0Wavelength for X ray), i.e. the relation curve of diffracted intensity and diffraction angle, again according to the interplanar distance of the residing angle calculation correspondence of the diffraction peak on the diffracting spectrum, the crystal structure of analysis of material.
Another kind of technology is energy dispersion X-ray diffraction (being called for short EDXRD), adopts white light x-ray bombardment sample, and detector is fixed on certain specific angle of diffraction 2 θ
0On.On this fixing angle, diffraction takes place and is detected the device reception different wavelength X (or photon energy E=12399/ λ) in different interplanar distance d, detector has the energy resolution ability, and the X ray that records is separated by its photon energy, is met diffraction formula 2dsin θ
0The diffracting spectrum of=12399/E, promptly the relation curve of diffracted intensity and photon energy can calculate interplanar distance equally according to the pairing photon energy of the diffraction peak on the collection of illustrative plates, analyzes the crystal structure of measured material.
But, above-mentioned technology all designs at the homogenous material sample.Because of the area of sample is bigger, need not consider the hot spot of X ray and the size of light intensity.
Along with the development of investigation of materials method, occurred at present with the synthetic material sample storehouse of combined method, promptly combined sample (claims again: material chip).It is a huge and intensive minute materials sample array.Small-sized (can be 1 square millimeter of area less than, the about 1 micron film of thickness) of each sample not only on this array, and the quantity of sample a lot (can reach 1000 or 10000), distance very near (can less than 0.1mm) between sample and the sample, type also can multiple (monocrystalline, polycrystalline, epitaxial films etc.).Therefore, when each sample on the material chip is carried out x-ray structure and constituent analysis, need to adopt the X-ray beam that hot spot is very little, intensity is very high,, shorten each sample needed analysis time, realize high-throughout combination X-ray analysis to improve sensitivity.At present, the analytical technology of having reported at combined sample has:
Synchrotron radiation combination X-ray analysis.Synchrotron radiation has very strong radiation flux at the X ray wave band, especially the brightness of third generation synchrotron radiation is high, adopt the ellipsoidal mirror of glancing incidence to focus on even sacrifice the light intensity of a magnitude, sacrifice one to two magnitude again, with aperture limited spot size, also also have enough light intensity to reach the demand of high throughput analysis.Unique deficiency is that synchrotron radiation is a big science engineering, is difficult to be adopted by common laboratory.
Perhaps, the θ of use angle chromatic dispersion method-2 θ interlock scan mode still.For example: the 1. D8DISCOVER WITH GADDS of Bruker company is to install the sample scan table additional and replace conventional slit-detector configuration with planar array detector on a conventional diffractometer (D8 DISCOVER).Because planar array detector can cover certain angle,, reach and θ-2 θ interlock scanning effect of equal value so can in certain scope, replace the rotation of sample.Its planar array detector is time-resolved multiwire chamber, has the certain energy resolution characteristic, but the gross-count rate of its planar array detector is only at per second about 20,000, the requirement that in fact can not reach high throughput analysis (is seen Bob B.H etc, XRD rapid screeningsystem for combinatorial chemistry, Denver X-ray conference 2000).2. the MicroX-200 of Intematix company.Adopt zone plate to focus on incident light, traditional θ-2 θ linked scan mode is measured diffraction spectra.Equip the solid energy-probe on the instrument and be used for constituent analysis.Owing to adopt θ-2 θ linked scan, each sample of perfect measurement approximately needs half an hour, material chip to integrated more than 1000 sample is analyzed, and needs 500 hours approximately, in fact also is impossible. the 3. parallel X-ray diffractometer of people's report such as M.Ohtania.The X ray that utilizes John's formula bent crystal that pointolite is sent is focused into the bar shaped laser spot of 0.1mm * 10mm on combined sample, so just can measure the diffraction spectra of the row sample that hot spot shines simultaneously.Also use two-dimensional array detector (CCD) image data, the incident light of convergence has the divergence of 2 degree, so once can measure 2 θ
BIt is the diffraction spectra in the 4 degree scopes.Because of its incident light divergence very big, so can only be used for monocrystalline or epitaxial film structures of samples measures, can't measure the polycrystalline sample and (see M.Ohtania, etc.Concurrent x-ray diffractometer for high throughput structural diagnosis of epitaxial thinfilms, Appl.Phys.Lett.79, P3594-3596,2001).
Though above-mentioned technology can be adopted by common laboratory, relative merits are arranged respectively: scheme advantage 1. is that mechanical interlock scanning, the shortcoming cancelled at a slow speed are that X ray does not focus on; Scheme advantage 2. is to have focused on X ray, but sweep velocity is slower; 3. scheme then can only be applicable to monocrystalline or extension sample.
Summary of the invention:
The objective of the invention is to provide a kind of simple to operate, measuring speed is very fast, the method and the device that can carry out high-throughout Measurement and analysis to the structure and the composition of various combined samples.
Technical solution of the present invention is as follows:
Method is: disperse the white light X ray is focused into quasi-parallel by X ray lens 3 the little convergent beams of white light X ray with what x-ray source 1 sent, focus is on the sample stage 7, the translation sample stage makes sample be positioned at this focus, receive the X ray and the sample emitted fluorescence X ray of diffraction from the sample then with energy-probe 9, be transferred to again and carry out data processing in the computing machine 12, obtain diffraction spectra and fluorescence spectrum, thereby obtain the structure and the composition information of combined sample.
Device is: by x-ray source 1, X ray lens 3, sample stage 7 and control circuit thereof, energy-probe 9 and metering circuit thereof, computing machine 12, instrument platform 13 compositions such as grade, computing machine by line respectively with sample stage and control circuit thereof, energy-probe and metering circuit thereof link to each other, x-ray source, the X ray lens, sample stage and control circuit thereof, energy-probe and metering circuit etc. thereof all place on the instrument platform, x-ray source and X ray lens are positioned on the same optical axis, form input path, energy-probe is positioned on the optical diffraction, wherein: described x-ray source is for dispersing white light X ray light source, the X ray lens are the little convergent lens of capillary bundle, energy-probe is a solid probe, sample stage is in the back focus place of the little convergent lens of X ray capillary bundle, energy-probe is aimed at the back focus of the little convergent lens of X ray capillary bundle, sample stage is provided with the translation displacement mechanism, specimen holder places on the sample stage, the surface of specimen holder is provided with sample and is in conplane XRF screen, camera 15 and the monitor 16 thereof that is positioned at the sample stage opposite also is set on the instrument platform, the camera sample plane on sample stage of focusing, monitor links to each other with camera by line; The software of storing or having solidified the displacement of control corresponding sample stage and institute's test sample product are carried out data acquisition and processing in the computing machine.
In the said apparatus, can also pinhole diaphragm 5 be set on the input path between X ray lens and the sample stage, X ray radome 14 is set on the optical diffraction between sample stage and the energy-probe.
That is to say that main points of the present invention focus on energy dispersion X-ray diffraction and X ray exactly and combine, and be applied in the structure of combined sample and the constituent analysis and go.
It is the difficult for a long time technical matters that realizes that X ray focuses on.At present, the little convergent lens of X ray capillary bundle is to focus on one of the most effective instrument of white light X ray, utilizes it can obtain the hot spot of the parallel or quasi-parallel X-ray beam that spot is little, brightness is high, is suitable for shining undersized sample.
Energy dispersion X-ray diffraction method itself is relatively low to requiring of dividing of instrument light path regulating, and need not rotate sample and detector in the measuring process, thereby can avoid having time saving potentiality owing to θ-2 θ rotates the location difficulty that needs minute adjustment to cause.
But because energy dispersion X-ray diffraction method requires incident light is parallel or the white light X ray of quasi-parallel, and the continuous spectrum white light X ray of common x ray generator is a little less than divergent state and the radiation, thereby can not directly use.Introducing by the little convergent lens of X ray capillary bundle, can make the diverging X-ray parallelization, and, because the X ray of directive different directions is put together, can also play simultaneously the effect of dwindling hot spot, increasing the unit area light intensity, the time saving potentiality of the method are come true.
Therefore, the advantage that energy dispersion X-ray diffraction and X ray capillary bundle is focused on both combines, just can utilize the fixing sample of the little convergent beams irradiating angle of white light X ray quasi-parallel that spot is little, brightness is high, like this, as long as just can analyze one by one fast to each small sample point on the combined sample by the translation sample stage.
But, will with above-mentioned both combine so that combined sample is measured, just must realize the system integration, the key issue that solves comprises the aligning of two light paths, the monitoring of incident light irradiation position, the automatic control of sample spot conversion and data acquisition and processing (DAP) thereof etc., otherwise the present invention just can not finish smoothly.
The concrete steps of Measurement and analysis method of the present invention are as follows:
That launches from x-ray source 1 disperses white light X ray 2, after X ray lens 3 converge, changes white light X ray 4 little convergent beams of quasi-parallel into, forms the incident light that spot is little, brightness is high; By the position of adjusting sample stage the focus of incident light is in the plane at sample surfaces place, by the translation sample stage focus is radiated on the corresponding sample point of combined sample 6 again; Then, go up the X ray of diffraction and energy-probe 9 and metering circuit thereof that sample emitted fluorescence X ray is on the diffraction locations receive from sample point, and be transferred in the computing machine 12 by its line, by computing machine 12 image data, and carry out atlas analysis through corresponding software, thereby obtain the structure and composition (element) information of sample.In the measuring process, the switching on the combined sample between each sample point is also controlled automatically, is realized by the control circuit and parallel the moving of displacement mechanism drive sample thereof of sample stage by the corresponding software in the computing machine 12.
The concrete structure of measurement analysis device of the present invention is as follows:
X-ray source 1, X ray lens 3, sample stage 7, energy-probe 9 etc. all place on the instrument platform 13, and preferably these parts are all placed in the suitable metal shell, the cover plate of housing should be convenient to open so that place sample and adjust each position component, then cover plate is covered the system that makes it to become an accurate sealing during measurement, to guarantee to measure without interruption and to avoid the leakage of X ray.X-ray source and X ray lens are positioned on the same optical axis, form input path, and described x-ray source is for dispersing white light X ray light source, and the X ray lens are the little convergent lens of capillary bundle.Energy-probe is positioned on the optical diffraction, and described energy-probe is a solid probe, and its metering circuit comprises power supply, signal amplifier and multichannel analyzer etc.X ray lens 3 and energy-probe 9 are shelved or are fixed on the instrument platform so that accurately locate by minute adjustment mechanism (for example three-dimensional universal minute adjustment frame) respectively.Sample stage 7 (for example Chang Yong three-dimensional accurate translation stage) then is fixed on the instrument platform, drive its three-dimensional translating displacement mechanism by stepper motor and control circuit thereof accurately locatees (perhaps, sample stage also can adopt the multidimensional governor motion with D translation function).Computing machine 12 adopts conventional computing machine (for example PC), can place the outer correct position place of instrument platform and housing thereof (using) as long as be convenient to the operator, be connected the software of storing or having solidified the displacement of control corresponding sample stage and institute's test sample product are carried out data acquisition and processing in the computing machine respectively with the control circuit of sample stage, the metering circuit of energy-probe by line.
Sample surfaces should be in the back focus place of X ray lens, can be provided with sample by 17 surfaces of the specimen holder on sample stage to be in conplane XRF screen 18, shows the spot size (the minimum place of hot spot is back focus) of X ray.Incident X-rays is pointed out by being arranged on the instrument platform and being positioned at the sample positioning monitoring system sample stage opposite, that comprise camera 15 and monitor 16 at the irradiation position on the combined sample.The camera sample surface on sample stage of focusing, monitor links to each other with camera by line, requires camera to have bigger magnification and short minimum photographic distance (for example: magnification is 1, and minimum photographic distance is 10cm).When the X-ray light spot on the video screen of from monitor, observing specimen holder, making position mark 19 on the monitor, owing to the position of camera is fixed, so the display position of incidence point on monitor also fixed.In measurement subsequently, the indicated position of this point be exactly sample point the position (because the direction of motion of translation stage is parallel with the sample face in measuring process, so mobile change of sample face and incident light intersection point locus that can not cause.Although variation has taken place in the sample spot that is on this intersection point).Also can adopt the computing machine that has video card to substitute monitor, camera 15 is linked to each other with computing machine by line.
If the sample spot of combined sample is small-sized, less than the formed spot size of incident light, shine a plurality of sample spot simultaneously for fear of incident light, can be according to installing sizeable pinhole diaphragm 5 additional on the input path of different sample spot sizes before sample stage, making incident light only shine a sample spot.Owing to adopted the capillary bundle focusing technology, the incident light of formation concentrates on spot center, even pinhole diaphragm has covered the X ray of a part of periphery, also can not have a strong impact on the demand of high throughput analysis.In addition, in order to reduce the influence of scattered light, metallic shield also can be installed before the detector block various spuious X ray.
In sum, incident light spot of the present invention is little, energy is high, can shine the sample spot, also unrestricted to the type of sample of very small dimensions, and sample does not need to rotate in the measuring process; Handoff procedure between sample spot and data acquisition can also be controlled automatically by computing machine; Sample diffraction spectra that records and fluorescence spectrum can reflect the structure and composition (element) information of sample.Thereby the present invention is simple to operate, and measuring speed is very fast; Can carry out high-throughout X-ray measurement analysis to the structure and the composition of various combined samples.
Description of drawings:
Accompanying drawing 1, the general structure synoptic diagram of measurement analysis device.
Accompanying drawing 2, sample position monitor synoptic diagram.
Accompanying drawing 3, the software flow pattern in the computing machine.
Accompanying drawing 4, examples measure collection of illustrative plates (detector is at the on-chip Ag film of the Si of position measurement collection of illustrative plates).
Accompanying drawing 5, examples measure collection of illustrative plates (detector is in the comparison of the on-chip Ag film of the Si collection of illustrative plates of two diverse locations measurements).
Embodiment:
X-ray source 1 employed x ray generator is the X-ray diffractometer BDX3200 type of company of Beida Jadebird, and the X-ray pipe is the Cu target X-ray tube of Dandong Ray Instrument Group Corp., model XJ10-60N.
Sample stage 7 and control circuit thereof adopt Beijing the stand upright accurate D translation platform of TSA50-C type, the SC3 controllor for step-by-step motor of Chinese light company.
Energy-probe 9 and metering circuit thereof adopt XR-100CR solid probe, the PX2T/CR power supply of U.S. Amptek company hold concurrently signal amplifier, MCA8000A multichannel analyzer.
Fixedly the minute adjustment frame of X ray lens 3 and energy-probe 9 is produced model ZJ-079B by Factory attached to Shanghai Univ. of Science ﹠. Technology.
The sample positioning monitoring system: the technical parameter of camera 15 is: magnification is 1, shooting distance is 10cm; Monitor 16 adopts common 10 cun black-and-white monitors.
The Unit Installation main points are as follows: determine that at first x-ray source sends the angular range of X-ray, place the little convergent lens of capillary bundle then and make the central lines of its axis and x-ray source transmitting boundary, then, move forward and backward little convergent lens and rotate luffing angle, x-ray source center (as the focal spot of X-ray pipe) is on the front focus f1 of lens.Next step exports a side with video screen at lens and seeks the back focus of lens (being the minimum place of projection hot spot): adjusts sample stage, the fixedly angle (θ of incident light and sample face
0), drive sample stage and move forward and backward, the back focus of lens is dropped in the plane at place, combined sample surface.Adjust detector to a suitable position, note making the back focus of detector over against lens, the detector center is fixed to the line of lens back focus and the angle between the incident light, is π-2 θ
0On optical diffraction, load onto metallic shield 14.Detector system and sample platform system connect with computing machine by cable 10,11.At of the requirement of sample spot size, appropriate pinhole diaphragm 5 is installed before the back focus of lens to the launching spot size; Diaphragm places between sample stage and the little convergent lens of capillary bundle, determines by hot spot brightness on the video screen on the observation sample frame and shape whether the installation of diaphragm is suitable.
The adjusting and the use of total system are as follows:
1. regulate the position and the angle of X ray lens 3, make the luminous point of x-ray source be positioned on the front focus of X ray lens 3.The concrete operations step is, at first X ray lens 3 are fixed on the minute adjustment frame, adjusting bracket is fixed on the instrument platform, near the back focus position of X ray lens 3, place the common X-ray detector (as NaI scintillator counter) of a window standard-sized sheet, add suitable attenuator before the detector,, make the reading maximum of detector by regulating three positions and two angles of minute adjustment frame, constitute input path with the position and the angle locking of adjusting bracket this moment;
2. remove above-mentioned detector and attenuator, sample stage is fixed on the instrument platform, sample face and input path are had a certain degree, drive sample stage, video screen 18 on the specimen holder 17 is on the position of detector of removing, can observe the X-ray light spot that video screen on focus on by camera 15 and monitor 16 this moment, move forward and backward video screen by driving sample stage, find the position of hot spot minimum, promptly being the back focus of X ray lens, also is the anchor point (can make respective markers 19 on the monitor screen) of sample measurement;
3. in specimen holder, place monocrystalline silicon piece (or other monocrystalline, also can as LiF, graphite etc., its a certain crystal face is parallel with the surface, monocrystalline silicon piece as (100) orientation), make the video screen on its surface and the specimen holder be in same plane, the translation sample stage is on the back focus of X ray lens monocrystalline silicon piece; Energy-probe is fixed on the minute adjustment frame, adjusting bracket is fixed on the instrument platform, make position of detector greatly on the position of optical diffraction, by regulating position of detector and angle, make the counting of detector reach maximum, this promptly is the position of optical diffraction, the position of lock adjustment frame and angle, constitute optical diffraction, at this moment, the detector center is π-2 θ to the line and the angle between the incident light of lens back focus
0
4. gather diffracting spectrum, according to the wavelength X of the X ray of silicon single crystal peak correspondence in the collection of illustrative plates
0Interplanar distance d with monocrystalline silicon
0, and diffraction formula 2d
0Sin θ
0=λ
0, demarcate angle of diffraction θ
0
But, for the polycrystalline sample,, thereby and do not require that incident light direction, sample surfaces, the strictness of emergent light direction satisfy direct reflection relation, its angle of diffraction θ because the angular range of its diffracted beam outgoing is very wide
0Can demarcate by the polycrystalline sample;
5. remove the monocrystalline silicon piece on the specimen holder, change material chip to be analyzed, drive translation stage, and observe, some positions (determining according to the automatic testing scheme that is provided with or selects) of material chip are positioned on the measurement point by camera and monitor;
6. by the computer control energy-probe, gather the data of certain hour.During this period of time, the x-ray photon that enters into detector forms the electric pulse that is proportional to photon energy at detector, and after amplifying, the height of pressing pulse separates, and is stored in the multichannel analyzer; After collection was finished, computing machine read the data of storing in the multichannel analyzer and obtains diffraction spectra and fluorescence Spectra, finished the data acquisition of a sample;
7. computer control translation stage, according to the testing scheme that is provided with or select next sample spot is moved to the sample anchor point, repeat above-mentioned steps 6., and the positional information of record sample, the diffraction spectra and the fluorescence Spectra of selected sample spot are finished by collection one by one on material chip.
Adopt said apparatus to test a material chip: 8 * 8 sample array is distributed on one inch square Si (100) monocrystal chip, and the some of them sample spot is the Ag polycrystalline film of about 1 micron thickness, 2.5mm * 2.5mm.In order to limit the diameter of incident beam, the pinhole diaphragm of 0.5 millimeter of diameter has been installed on light path.Test process shows that the auto-control software operation of this complete equipment is normal, can realize that promptly sample stage moves the robotization of control and data acquisition.
Fig. 4 is exactly the data collection of illustrative plates that collects from one of them Ag sample spot, and this collection of illustrative plates is analyzed as can be known:
1. the diffraction peak (400) of main diffraction peak (111), (200), (220), (311), (222) and the Si monocrystal chip of Ag polycrystalline film all appears in the collection of illustrative plates, and this confirms that this platform can carry out the qualitative analysis of structure.
The L that 2. can also see Ag in spectrum is fluorescence peak (L of Ag is that fluorescent line is superimposed owing to energy is close), illustrates that this platform can carry out constituent analysis.
Certainly, collect such spectrum, how carrying out qualitative analysis also is the problem that needs are considered.Explanation at this point below.
The energy of the characteristic spectral line of every kind of element (fluorescence peak) determines that the variation with detector position does not change, and according to the Bragg diffraction formula as can be known, the position of lattice diffraction peak is with position of detector (2 θ
0) closely-related.Like this, the tester can with two detectors in different positions (i.e. 2 θ
0Different) gather collection of illustrative plates simultaneously, by contrast two collection of illustrative plates distinguish fluorescence peak and diffraction peak (peak position constant be fluorescence peak, variation be diffraction peak); Each is measured once in different positions perhaps to use a detector, contrasts two collection of illustrative plates then.
Fig. 5 is exactly the Ag film that detector records two different positions--the contrast of Si (100) substrate collection of illustrative plates.Solid line and dotted line are used for identifying this two collection of illustrative plates respectively.Detector position 2 θ when gathering the dotted line collection of illustrative plates
0Big when gathering the solid line collection of illustrative plates, when gathering the solid line collection of illustrative plates, detector position 2 θ
0=40 °; When gathering the dotted line collection of illustrative plates, detector position 2 θ
0=50 °.
Contrast the position at peak in two collection of illustrative plates, the position at a, b, three peaks of c does not change in the spectrum as can be seen, and explanation is a fluorescence peak, tables look-up according to the X-ray energy of peak value correspondence, and they are respectively as can be known, and the L of a:Ag is a fluorescence peak, the K of b:Cu
αThe peak, the K of c:Cu
βThe peak.A in the dotted line collection of illustrative plates
1, B
1, C
1The position at three peaks obviously changes, and explanation is a diffraction peak, corresponding to the A in the solid line collection of illustrative plates
2, B
2, C
2The peak, residing position 2 θ of detector according to the X-ray ENERGY E ι of peak value correspondence and when measuring
0, according to the interplanar distance di that the Bragg diffraction formula can be calculated the diffraction peak correspondence, tabling look-up as can be known, they are respectively (400) diffraction peaks of (111), (200) diffraction peak and the Si substrate of Ag.
Above description of test this system can carry out structure, constituent analysis to combined sample, and realized the robotization of the control of whole sample array test, data acquisition.
In this embodiment, the acquisition time of each collection of illustrative plates is about 10 minutes.This is that its actual power that uses is 720W (36KV, 20mA) because what use is Cu target X-ray pipe, and in the emission spectrum of copper the continuous spectrum composition a little less than.If (power that changes target X-ray pipe can reach more than the 10KW to use commentaries on classics target fine focus heavy element target X-ray pipe; Heavy (element) target---such as strong than Cu of continuous spectrum composition in the emission spectrum of W), the double detector system, the Measuring Time of each sample spot can shorten in one minute, reached the effect of quick measurement.
Claims (3)
1, a kind of method that the structure and the composition of combined sample are carried out Measurement and analysis, it is characterized by: disperse the white light X ray is focused into quasi-parallel by X ray lens (3) the little convergent beams of white light X ray what x-ray source (1) sent, focus is on the sample stage (7), the translation sample stage makes sample be positioned at this focus, use energy-probe (9) to receive the X ray and the sample emitted fluorescence X ray of diffraction from the sample then, be transferred to again in the computing machine (12) and carry out data processing, obtain diffraction spectra and fluorescence spectrum, thereby obtain the structure and the composition information of combined sample.
2, a kind of device that the structure and the composition of combined sample are carried out Measurement and analysis is characterized by: comprise x-ray source (1), X ray lens (3), sample stage (7) and control circuit thereof, energy-probe (9) and metering circuit thereof, computing machine (12), instrument platform (13); Computing machine links to each other with sample stage and control circuit, energy-probe and metering circuit thereof respectively by line, x-ray source, X ray lens, sample stage and control circuit, energy-probe and metering circuit thereof all place on the instrument platform, x-ray source and X ray lens are positioned on the same optical axis, form input path, and energy-probe is positioned on the optical diffraction; Described x-ray source is for dispersing white light X ray light source, the X ray lens are the little convergent lens of capillary bundle, energy-probe is a solid probe, sample stage is in the back focus place of the little convergent lens of X ray capillary bundle, energy-probe is aimed at the back focus of the little convergent lens of X ray capillary bundle, sample stage is provided with the translation displacement mechanism, and specimen holder places on the sample stage, and the surface of specimen holder is provided with sample and is in conplane XRF screen; Camera (15) and the monitor (16) thereof be positioned at the sample stage opposite are set on the instrument platform, the camera sample plane on sample stage of focusing, monitor links to each other with camera by line; The software of storing or having solidified the displacement of control corresponding sample stage and institute's test sample product are carried out data acquisition and processing in the computing machine.
3, device as claimed in claim 2 is characterized by: pinhole diaphragm (5) is set on the input path between X ray lens and the sample stage; X ray radome (14) is set on the optical diffraction between sample stage and the energy-probe.
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