CN101776620B - Bent crystal light splitting device of wavelength dispersion X-fluorescence spectrograph and operating method thereof - Google Patents
Bent crystal light splitting device of wavelength dispersion X-fluorescence spectrograph and operating method thereof Download PDFInfo
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- CN101776620B CN101776620B CN200910068795.9A CN200910068795A CN101776620B CN 101776620 B CN101776620 B CN 101776620B CN 200910068795 A CN200910068795 A CN 200910068795A CN 101776620 B CN101776620 B CN 101776620B
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Abstract
The invention relates to a bent crystal light splitting device of a wavelength dispersion X-fluorescence spectrograph, comprising a front-slit conduit, a light splitting box body, a crystal bracket, a rear-slit conduit and a detector. The operating method comprises the following steps of: affixing a crystal film on the crystal bracket which is in accordance with the overall-focusing and logarithmic spiral special curve via calculation, fixing the crystal film in the light splitting box body, and regulating the angle of the crystal bracket to be consistent with a theoretical curve, wherein the front-slit conduit, an inner cavity of the light splitting box body, the crystal, the crystal bracket and the rear-slit conduit form a light splitting path; and connecting the detector with the rear-slit conduit, and performing quantified detection on the characteristic X ray of a certain element selected by the light splitter. The invention has the advantages that the structural design of a wedge-shaped inner cavity and a rear opening reduces the amount of the scattered surface of the X ray, is beneficial to lowering the intensity of background signals of instrument detection data, reducing the inside and outside dimension of the light splitter and arranging vacuum seal and the light splitter; besides, the seal between the light splitter and a vacuum chamber is double radial shaft seal, thereby the positioning precision of the light splitter and the vacuum chamber is improved.
Description
(1) technical field:
The present invention relates to a kind of X ray crystal light splitting and method of work thereof, especially a kind of bent face crystal light splitting and method of work thereof of wavelength dispersion X-fluorescence instrument, it is the vitals of X-ray analysis wavelength dispersion X-fluorescence instrument, and light-dividing device structure and performance directly determine the quality of spectrometer performance.
(2) background technology:
Wavelength dispersion X-fluorescence instrument is quantitative test material chemical analysis exact instrument, is widely used in the fields such as building materials, metallurgy, environmental protection and scientific research.X ray crystal light splitting is the most crucial parts of nuclear instrument.Its principle of work (as Fig. 1), the secondary x rays with each component elemental characteristic spectral line that sample is inspired by X-ray tube is collected in optical splitter by prime slit, in optical splitter, place the crystal of a specific lattice spacing, when the optical path length of incident X-rays and the angle of incident crystal meet Bragg equation, (in 2dsin θ=λ formula, d is interplanar distance; Angle between θ incident ray and diffraction surfaces; λ is the wavelength of characteristic X-ray) time, just can obtain the monochromatic characteristic X-ray of certain element with the specific angle and distance of plane of crystal place, on this position, X-ray detector is set, X ray light energy signal is transferred to electric signal and carries out accurate quantitative test, detect the content of certain element in sample.
(3) summary of the invention:
The object of the invention is to design a kind of bent face crystal light splitting and method of work thereof of wavelength dispersion X-fluorescence instrument, it adopts wedge structure and double curvature method or equiangular spiral method bent face crystal to carry out wavelength dispersion, is that a kind of spectroscopical effeciency is high, noise background is low, structure is simple and direct and the optical splitter formation of the reliable novel high-performance of vacuum seal.
Technical scheme of the present invention: a kind of bent face crystal light splitting of wavelength dispersion X-fluorescence instrument, is characterized in that it comprises front slit conduit, light splitting box body, crystal bracket, rear slit conduit and detector; The incident end of light splitting box body is that the entrance port of light path is provided with front slit conduit, and the exit end of light splitting box body is that the exit portal of light path is sealed and installed with rear slit conduit; The light path axle center of said crystal bracket is fixed in light splitting box body according to bearing pin, on crystal bracket, has crystal film, and the light path axle center of crystal bracket is taking bearing pin as axis of rotation; Said rear slit conduit and detector are sealing and install.
The light path shape that the optical splitter inner chamber that above-mentioned said front slit conduit, light splitting box body and rear slit conduit form calculates according to the method in patent work principle of the present invention is processed into wedge shape.
Dual radially O-ring seals before the locating surface that above-mentioned said light splitting box body is installed according to optical splitter location and vacuum chamber and the sealing of light splitting vacuum chamber mounting hole are installed, and are and are fixed connection according to the screw of mounting hole periphery.
The locating surface that above-mentioned said optical splitter location and vacuum chamber are installed and the light path axle center of crystal bracket, in the same face, are easy to the distance of measurement and positioning face and axle center hole, and the processing of this position and installation accuracy are the keys of optical splitter effect.
Above-mentioned said crystal bracket curved surface is the coordinate data calculating according to the method in patent work principle of the present invention, is processed by numerically-controlled machine; Axle center hole is left in light path center in crystal bracket two sides, and bearing pin is penetrated by light-splitting box both sides, and crystal bracket is fixed on light splitting box body, and crystal bracket can rotate along bearing pin; Bearing pin is according to screw thread and dual O-ring seals and light splitting box body sealing installation.
The opening that crystal is installed is left in the bottom of above-mentioned said light splitting box body, and opening part is sealed and installed with bonnet according to O-ring seals I; Crystal bracket angular setting push rod and back-moving spring are installed on said bonnet, and crystal bracket angular setting push rod is sealing according to O-ring seals II and bonnet and installs; Crystal bracket angular setting push rod and back-moving spring are connected to the two ends of crystal bracket.Between light splitting box body and bonnet, be connected according to screw.
The slit width of above-mentioned said front slit conduit and rear slit conduit can be changed according to the needs of different sample elements.
Above-mentioned said front slit conduit and light splitting box body are in together in vacuum, without sealing, only need screw to connect; Rear slit catheter proximal end is installed with screw sealing according to O-ring seals III and light splitting box body, and rear end and detector are installed with screw sealing according to O-ring seals IV.
A method of work for the bent face crystal light splitting of wavelength dispersion X-fluorescence instrument, is characterized in that it comprises the following steps:
(1) according to double curvature method or equiangular spiral method design light splitting optical path, calculate in light path the coordinate for the segment of curve of light splitting, and press curvillnear coordinate worked crystal bracket, and the crystal film processing is sticked on crystal bracket, plane of crystal and the light path curve calculating are matched;
(2) in crystal bracket being fixed in light splitting box body with bearing pin, then cover bonnet, the back-moving spring being provided with bonnet and crystal bracket angle adjustment lever are withstood the crystal bracket back side, by their acting in conjunction, turn crystal bracket is adjusted push rod, simultaneously by the effect of back-moving spring, adjust within the specific limits the angle of crystal bracket, in the time that electric signal is the highest, think that crystal angle conforms to calculated value, live adjustment hole with wax seal;
(3) light-splitting box intracoelomic cavity is processed into wedge shape according to the shape of light path, to meet passing through of the required X-fluorescence of light splitting, at utmost reduce scattering and the reflection of X ray simultaneously, shelter from the X ray of other harmful scatterings and reflection simultaneously, accomplish the interior physical dimension minimum of optical splitter simultaneously, improve vacuum seal performance;
(4) slit conduit before the incident end of light splitting box body is loaded onto, slit conduit after the exit end of light splitting box body is loaded onto, like this, front slit conduit, light splitting box body, crystal bracket, crystal, rear slit conduit form light splitting optical path;
(5) detector is connected with rear slit conduit, characteristic X-ray through crystal light splitting focusing is irradiated on detector, transfer light signal to electric signal, thereby the characteristic X ray strength of certain element that optical splitter is sub-elected carries out quantitative measurment, can detect like this content of certain element in sample;
(6) in optical splitter, to keep vacuum state, requiring has good sealing between every two parts that are connected, make O-ring seals I, O-ring seals II and dual radially O-ring seals respectively with sealing surface good contact, and according to screw in compression, guarantee the vacuum seal of light-dividing device;
(7) optical splitter requires there is good location precision between every two parts that are connected, to guarantee that the physics light path size that optical splitter forms conforms to abstract optical dimensions; This reaches designing requirement with regard to the dimensional accuracy that needs each parts, and when mounted simultaneously, each locating surface will be in conjunction with closely, and according to screw in compression; Place locating surface is rigidity, does not move with the O-ring seals distortion of sealing use; Wherein the location dimension of most critical is the distance size of the installation locating surface of crystal axis center and optical splitter and vacuum chamber, and this size should be easy to processing and measure;
(8) the incident end of the light splitting box body of light-dividing device inserted to vacuum chamber together with front slit conduit, junction is sealed with dual radially O-ring seals, and the locating surface of light-dividing device and vacuum chamber is compressed, crystal and crystal bracket are fixed on the crystal axis place of light splitting box body with bearing pin, first-class bonnet, after rear slit and detector are reliably connected with light-splitting box, the condition that light-dividing device has carried out light splitting with regard to having possessed secondary x rays that sample excitation is gone out.
Principle of work of the present invention: the present invention adopts double curvature method or equiangular spiral method bent face crystal to carry out wavelength dispersion;
Double curvature method, claims again total focus method: as Fig. 2, first single crystal ingot is ground to the thin slice that radius-of-curvature is R, makes the atomic plane in this thin slice all parallel with the tangent plane of crystal mid point; And then by this wafer curve taking O ' as the center of circle, R/2 is the cylinder of radius; So, wherein reflect that atom is all curved taking O as the center of circle, R is the cylinder of radius; As seen from Figure 1, the tangent plane uu of A, B and C tri-point atom faces is vertical with OC with OA, OB respectively; In Fig. 1, AP=L=n λ R/2d=Rsin θ meets Bragg condition; In like manner each incident ray all meets cloth brace members, and strictly focuses on P point; In the jewelry making practice of crystal, be generally the crystal mould of fixing several R values, adjust the distance L value of slit to germ nucleus for different diffraction angle, make light path meet Bragg condition;
Fig. 3 is the index path as an example of Elements C a example, make R/2=100mm, L=OA, circular arc line will pass through O and A point simultaneously, and P is the symmetric points of O with respect to A, making O is front slit point, A is germ nucleus point, and P is rear slit point, and single crystal ingot is ground to the thin slice that radius-of-curvature is R, be bonded at the metal support that intrados is R/2, and make crystal bracket; Optical splitter and crystal bracket have just formed a complete light splitting optical path like this, therefore just can utilize the special construction of twice bending intracell of crystal to carry out X ray light splitting with the optical splitter of this structure;
Equiangular spiral method, claims again logarithmic spiral method: the polar coordinates mathematic(al) representation of equiangular spiral is: ρ=Ae ψ ctg θ, and curve is as Fig. 2: its mathematical definition is: on limit pts and curve, the angle of the tangent line of the line of any point P and P point place curve is all θ; We utilize this character of equiangular spiral, will in formula θ, be taken as Bragg angle θ; Limit is entrance slit; Crystal only need simply grind into plane lamina, is posted on the crystal bracket that is processed into equiangular spiral shape; Each light being irradiated on crystal all becomes Bragg angle with crystal like this; Be intersected in a very little region through the X ray of diffraction, instead of complete double curvature, but focusing range is very little, and high a lot of more than the intensity of flat crystal;
Front slit is to distance p, the crystal effective diameter D at analyzing crystal center, sample is interrelated to tetra-parameters of effective length S of entrance slit distance 1 and crystal, light path is more short better, be that l+p is more short better, but l is less, can make crystal length longer, light-splitting box cavity diameter strengthens, the making of crystal is difficulty all the more, and cost is also higher; Because vacuum chamber can not be too little, so p value also will be subject to the restriction of structure; Therefore, in design process, comprehensive above various factors, repeatedly optimize and calculate, finally determine crystal effective diameter D, ray taking-up angle
sample to entrance slit apart from l, front slit the distance p to analyzing crystal center
0etc. parameter as basic experience parameter;
The surface curve of crystal bracket will to drop on equiangular spiral that section consistent with light path; Through how much coordinate figures that calculate on this section of curve enough, to export to numerically controlled wire cutting machine crystal bracket surface is processed, logarithm crystal is made the crystal that one deck is very thin and is bonded on crystal bracket;
The crystal axle center of light-dividing device (Fig. 5) is that bearing pin place is the PO point of Fig. 4, front slit conduit 13 centers are pts point in Fig. 4, the F point that rear slit conduit 16 centers are Fig. 4, optical splitter and crystal bracket have just formed a complete light splitting optical path like this, therefore just can utilize the special mathematical characteristic of equiangular spiral to carry out X ray light splitting with the optical splitter of this structure;
Optical splitter adopts wedge structure, as Fig. 5: X ray light path 12 is wedge shapes, and therefore, optical splitter inner chamber is tightly around X ray light path design wedgewise.
Superiority of the present invention is: a, bent face crystal have focussing force to X ray, enters high 2 orders of magnitude of X ray strength ratio flat crystal light splitting of detector after focusing; B, the light splitting of bent face crystal are without the necessary front and back of flat crystal light splitting collimating apparatus, and front and back collimating apparatus has into the decay of 2 orders of magnitude to X ray; The physical dimension of the front slit of c, the light splitting of bent face crystal is little, can draw closer together to sample, and farthest reduce X ray decay in the air; D, the light splitting of bent face crystal crystalline size used is less, is conducive to growth and the processing of crystal; E, optical splitter inner chamber except for light path by and space there is no unnecessary space, reduce to the full extent the burden of vacuum system; F, wedge shape inner chamber have reduced the quantity of the face of X ray scattering to the full extent, are conducive to the intensity of the background signal of lowering apparatus detection data; The structural design of g, wedge shape inner-cavity structure and after-opening, reduces the aperture area of optical splitter to the full extent, is conducive to vacuum seal; The size of the relative optical splitter datum clamp face in crystal installation shaft center of h, wedge shape inner-cavity structure is easy to measure in machining, can greatly improve the precision of machining, is also convenient to the inspection of optical splitter section; I, optical splitter profile are completely parallel with inner chamber, and physical dimension minimum can increase more point session for fixing road X-fluorescence spectrometer in the situation that of vacuum chamber constancy of volume; The Installation and Debugging of j, optical splitter all complete on bonnet, for fixing road X-fluorescence spectrometer, carry out Installation and Debugging very convenient from this angle; Sealing between k, optical splitter and vacuum chamber changes double radial shaft sealing into by traditional butt-end packing, greatly improve the positioning precision of optical splitter and vacuum chamber, stopped traditional butt-end packing optical splitter simultaneously and be out of shape due to seal during use the phenomenon of the data drift causing; Front slit conduit in l, this device and the slit width of rear slit conduit can be changed according to the needs of different sample elements.
(4) brief description of the drawings:
Fig. 1 is flat crystal diffraction principle figure.
Fig. 2 is total focus crystal diffraction schematic diagram.
Fig. 3 is total focus light splitting optical path figure.
Fig. 4 is logarithm spiral shell light splitting optical path figure.
Fig. 5 is the structural representation of the bent face crystal light splitting of the related a kind of wavelength dispersion X-fluorescence instrument of the present invention.
Wherein, 1 is O-ring seals I, and 2 is O-ring seals II, 3 is bonnet, and 4 is crystal bracket angular setting push rod, and 5 is back-moving spring, 6 is light splitting box body, and 7 is crystal bracket, and 8 is bearing pin, 9 is crystal film, and 10 is optical splitter location and the locating surface of vacuum chamber installation, and 11 is dual radially O-ring seals, 12 is light path, and 13 is front slit conduit, and 14 is O-ring seals III, 15 is O-ring seals IV, and 16 is rear slit conduit, and 17 is detector.
(5) embodiment:
Embodiment: a kind of bent face crystal light splitting (seeing Fig. 5) of wavelength dispersion X-fluorescence instrument, is characterized in that it comprises front slit conduit 13, light splitting box body 6, crystal bracket 7, crystal bracket angular setting push rod 4, back-moving spring 5, bonnet 3, rear slit conduit 16 and detector 17; Wherein, the inner chamber of light splitting box body 6 is processed into wedge shape according to the shape of light path 12, the incident end end of light splitting box body 6 is that the entrance port of light path 12 is provided with front slit conduit 13, the exit end of light splitting box body 6 is that the exit portal of light path 12 is sealed and installed with rear slit conduit 16 according to O-ring seals III14, the opening that crystal is installed is left at the middle part of light splitting box body 6, and opening part is sealed and installed with bonnet 3 according to O-ring seals I1; Crystal bracket angular setting push rod 4 and back-moving spring 5 are installed on said bonnet 3, and crystal bracket angular setting push rod 4 is sealing according to O-ring seals II 2 with bonnet 3 and installs; The light path axle center of said crystal bracket 7 is fixed in light splitting box body 6 according to bearing pin 8, on crystal bracket 7, there is crystal film 9, the two ends of crystal bracket 7 connect respectively crystal bracket angular setting push rod 4 and back-moving spring 5, and the light path axle center of crystal bracket 7 is taking bearing pin 8 as axis of rotation; Said rear slit conduit 16 is sealing according to O-ring seals IV15 and detector 17 and installs.
The slit width of above-mentioned said front slit conduit 13 and rear slit conduit 16 can be changed according to the needs of different sample elements.(seeing Fig. 5)
Above-mentioned said front slit conduit 13 is connected according to screw with light splitting box body 6 and is arranged in light splitting vacuum chamber; The dual radially O-ring seals 11 at locating surface 10 places that said light splitting box body 6 is installed according to optical splitter location and vacuum chamber is installed with the sealing of light splitting vacuum chamber mounting hole, and is and is fixed connection according to the screw of mounting hole periphery.(seeing Fig. 5)
Between above-mentioned said light splitting box body 6 and bonnet 3, be connected according to screw.(seeing Fig. 5)
Above-mentioned said rear slit conduit 16 is connected according to screw with light splitting box body 6 and detector 17 respectively.(seeing Fig. 5)
Above-mentioned said detector 17 is flow-gas proportional counter.(seeing Fig. 5)
A method of work for the bent face crystal light splitting of wavelength dispersion X-fluorescence instrument, is characterized in that it comprises the following steps:
(1) according to double curvature method or equiangular spiral method design light splitting optical path, calculate in light path the coordinate for the segment of curve of light splitting, and press curvillnear coordinate worked crystal bracket 7, the crystal film processing is sticked on crystal bracket 7, plane of crystal and the light path curve calculating are matched;
(2) with bearing pin 8 by crystal bracket 7 be fixed on light splitting box body 6 interior in, then cover bonnet 3, the back-moving spring 5 being provided with bonnet and crystal bracket angle adjustment lever 4 are withstood crystal bracket 7 back sides, by their acting in conjunction, turn crystal bracket is adjusted push rod 4, simultaneously by the effect of back-moving spring 5, adjust within the specific limits the angle of crystal bracket, in the time that electric signal is the highest, think that crystal angle conforms to calculated value, live adjustment hole with wax seal;
(3) light splitting box body 6 inner chambers and crystal bracket 7 form light splitting optical path;
(4) slit conduit 13 before the incident end of light splitting box body 6 is loaded onto, slit conduit 16 after the exit end of light splitting box body 6 is loaded onto;
(5) detector 17 is connected with rear slit conduit 16;
(6) make O-ring seals I 1, O-ring seals II 2 and dual radially O-ring seals 11 respectively with sealing surface good contact, tighten housing screw, guarantee the vacuum seal of light-dividing device;
(7) the incident end of the light splitting box body 6 of light-dividing device inserted to vacuum chamber together with front slit conduit 13, junction is sealed with dual radially O-ring seals 11, and the locating surface of light-dividing device and vacuum chamber 10 is compressed, light-dividing device starts sample to carry out light splitting.
Claims (7)
1. a bent face crystal light splitting for wavelength dispersion X-fluorescence instrument, is characterized in that it comprises front slit conduit, light splitting box body, crystal bracket, rear slit conduit and detector; The incident end of light splitting box body is that the entrance port of light path is provided with front slit conduit, and the exit end of light splitting box body is that the exit portal of light path is sealed and installed with rear slit conduit; The light path axle center of said crystal bracket is fixed in light splitting box body according to bearing pin, on crystal bracket, has crystal film, and the light path axle center of crystal bracket is taking bearing pin as axis of rotation; Said rear slit conduit and detector are sealing and install; The optical splitter inner chamber that said front slit conduit, light splitting box body and rear slit conduit form is processed into wedge shape according to light path shape.
2. according to the bent face crystal light splitting of the said a kind of wavelength dispersion X-fluorescence instrument of claim 1, it is characterized in that dual radially O-ring seals and light splitting vacuum chamber mounting hole sealing installation before said light splitting box body is according to the locating surface of optical splitter location and vacuum chamber installation, and be and be fixed connection according to the screw of mounting hole periphery.
3. according to the bent face crystal light splitting of the said a kind of wavelength dispersion X-fluorescence instrument of claim 1, it is characterized in that said optical splitter location and the locating surface of vacuum chamber installation and the light path axle center of crystal bracket are in the same face.
4. according to the bent face crystal light splitting of the said a kind of wavelength dispersion X-fluorescence instrument of claim 1, it is characterized in that said crystal bracket curved surface is the coordinate data calculating according to the method in patent work principle of the present invention, processed by numerically-controlled machine; Axle center hole is left in light path center in crystal bracket two sides, and bearing pin is penetrated by light-splitting box both sides, and crystal bracket is fixed on light splitting box body, and crystal bracket can rotate along bearing pin; Bearing pin is according to screw thread and dual O-ring seals and light splitting box body sealing installation.
5. according to the bent face crystal light splitting of the said a kind of wavelength dispersion X-fluorescence instrument of claim 1, it is characterized in that the opening that crystal is installed is left in the bottom of said light splitting box body, opening part is sealed and installed with bonnet according to O-ring seals I; Crystal bracket angular setting push rod and back-moving spring are installed on said bonnet, and crystal bracket angular setting push rod is sealing according to O-ring seals II and bonnet and installs; Crystal bracket angular setting push rod and back-moving spring are connected to the two ends of crystal bracket; Between light splitting box body and bonnet, be connected according to screw.
6. according to the bent face crystal light splitting of the said a kind of wavelength dispersion X-fluorescence instrument of claim 1, it is characterized in that the slit width of said front slit conduit and rear slit conduit can be changed according to the needs of different sample elements.
7. according to the bent face crystal light splitting of the said a kind of wavelength dispersion X-fluorescence instrument of claim 1, it is characterized in that said front slit conduit and light splitting box body are in together in vacuum, without sealing, only need screw to connect; Rear slit catheter proximal end is installed with screw sealing according to O-ring seals III and light splitting box body, and rear end and detector are installed with screw sealing according to O-ring seals IV.
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