CN109374659A - A kind of localization method of short wave length X-ray diffraction test sample - Google Patents
A kind of localization method of short wave length X-ray diffraction test sample Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000002441 X-ray diffraction Methods 0.000 title claims abstract description 37
- 230000004807 localization Effects 0.000 title claims abstract description 9
- 230000005540 biological transmission Effects 0.000 claims abstract description 27
- 239000002356 single layer Substances 0.000 claims abstract description 9
- 238000001228 spectrum Methods 0.000 claims description 29
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- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 229910001069 Ti alloy Inorganic materials 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 5
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- 238000010586 diagram Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
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- 238000004458 analytical method Methods 0.000 description 2
- 230000001815 facial effect Effects 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001683 neutron diffraction Methods 0.000 description 2
- 238000009659 non-destructive testing Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000005469 synchrotron radiation Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
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Abstract
The present invention provides a kind of localization method of short wave length X-ray diffraction test sample, step includes: to be fixedly installed in test sample on the sample stage of short wave length X-ray diffraction device；The a certain test position of test sample is chosen as datum mark；The Y axis coordinate Y of test sample datum mark is irradiated or obtained using the method that test penetrates the X-ray transmission intensity distribution of sample datum mark using laser beamS, Z axis coordinate ZSWith X axis coordinate XS；Very according to coordinate XS、YS、ZSWith the scale coordinate relationship of test sample, calculate the three-dimensional coordinate for determining the other detected parts of test sample, determining detected part coordinate is calculated by moving to the X, Y, Z axis of sample stage, so that test sample detected part to be positioned to the center of circle of short wave length X-ray diffraction instrument circle.The present invention solves the orientation problem of the wall thickness such as single layer flat samples, hollow sample, the hollow wall thickness sample interior test position such as not, can be realized the accurate positioning to various test sample test positions.
Description
Technical field
The present invention relates to X-ray diffraction detection techniques, and in particular to a kind of positioning of short wave length X-ray diffraction test sample
Method.
Background technique
Neutron diffraction techniques, high energy Synchrotron Radiation Technology and short wave length X-ray diffraction technology may serve to detection material
Inside workpiece residual stress, texture and object are equal, wherein short wave length X-ray diffraction technology is sent out using heavy metal target X-ray tube
Strong penetrability characteristic X-ray (such as WK outα、UKα、WKβDeng), the directional light constituted using incident collimator and reception collimator
Road (intersection point of incident ray and diffracted ray is the spatial position of sample test point, i.e. the center of circle of short wave length X-ray diffraction instrument circle), nothing
The diffracted intensity and diffraction spectra of the center point substance of loss measurement diffractometer circle.
CN100485373C discloses a kind of short wave length X-ray diffraction measuring device, including X-ray tube, incident diaphragm, work
Make platform, receive slit, angular instrument, detector, energy analyzer, X-ray tube and detector are located at workbench and being tested thereon
Workpiece two sides carry out tomoscan measurement to measured workpiece using short wave length X-ray diffraction transmission beam method；Receive slit, detector
It is fixed on angular instrument, the synchronous measured workpiece measured point on using workbench is rotated as the center of circle, this measured point is located at angular instrument
In shaft；Angular instrument is fixed on a platform；Workbench is fixed on angular instrument, or is fixed on platform；X-ray tube is solid
Due on angular instrument, or it is fixed on platform；Incident diaphragm is fixed on angular instrument, or is fixed on platform, or is fixed on X
Fixture on ray tube；Incident diaphragm exports or on angular instrument circumference, or in angular instrument circumference: the tested work on workbench
Part makees the translation of X, Y, Z three-dimensional respectively with workbench or rotates Ψ angle around angular instrument shaft or make X, Y, Z, Ψ linkage.
It is as follows using short wave length X-ray diffraction technology measuring device measurement inside workpiece residual stress, the method for object phase: selective radiation
With diffraction test parameter, the center of circle including tube voltage, tube current, diaphragm and slit system and angular instrument circle to radiation detector
Or distance of position sensitive detector etc.；Workpiece measured point is placed in the center of circle of angular instrument circle by computer control；Computer control is surveyed
Measure diffraction spectra；As needed, X, Y, Z three-dimensional direction moving are made by computer control workbench or is rotated around angular instrument shaft, just
The diffraction spectra at any point and its any angle Ψ in workpiece can be measured；Data processing is carried out by computer, acquires each point object phase, residual
Residue stress parameter and its distribution.Compared to neutron diffraction techniques and high energy Synchrotron Radiation Technology, short wavelength X is carried out using the device
Ray diffraction techniques detection has many advantages, such as that at low cost, maintenance cost is few.However, simultaneously based on the device and other existing literatures
Test position a certain inside test sample can be accurately placed in the positioning side in the center of circle of short wave length X-ray diffraction instrument circle
Method.
Summary of the invention
The purpose of the present invention is to provide a kind of localization methods of short wave length X-ray diffraction test sample, and this method can
Guarantee that sample test position is located at the center of circle of diffractometer, enable using when the test of short wave length X-ray diffraction instrument accurately without
Damage detects the diffraction information at surveyed position, equal to analyze test sample internal stress, texture and object.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of localization method of short wave length X-ray diffraction test sample, steps are as follows:
Step 1: test sample being fixedly installed on the sample stage of short wave length X-ray diffraction device；
Step 2: choosing a certain test position of test sample as datum mark；
Step 3: the method for the X-ray transmission intensity distribution irradiated using laser beam or penetrate sample datum mark using test is obtained
Take the Y axis coordinate Y of test sample datum markS；
Wherein, for single layer flat samples and hollow same wall thickness sample datum mark coordinate YSAcquisition methods are as follows: by sample
Clamping keeps the surface normal at tested position parallel with X-ray incident direction on sample stage, is directed toward diffraction using X-direction
The laser of the round heart of instrument is positioned, and the Y axis coordinate Y of datum mark is obtainedS；
The hollow specimen datum mark Y axis coordinate acquisition methods different for wall thickness are as follows: first one piece of thickness of clamping is equal on sample stage
Even plate sample (such as aluminium sheet), and make the planar surface normal parallel with X-ray incident direction, adjust the voltage of X-ray tube
And electric current, guarantee that x-ray photon counts the saturation count for being much smaller than detector when transmission；Then (of the invention nearby in 2 θ=0 °
Within the scope of ± 5 ° nearby referred to as known to those skilled in the art), the x-ray count intensity of 2 θ scanning surveys transmission is along 2 θ
The curve of distribution, carries out curve fitting, and calculates 2 angle position θ, 2 θ for determining max transmissive intensity0, and place the detector 2 θ0,
Place the detector the angle position of face X source；Plate is removed again, the different hollow sample of clamping wall thickness on sample stage
Product, and make the surface normal at tested position parallel with X-ray incident direction, adjust the voltage and current of X-ray tube, Y-axis
The x-ray photon count intensity of scanning survey transmission carries out the Smoothing fit of curve, finally combines along the distribution curve of coordinate Y
Known thickness of sample variation characteristic chooses the datum mark of test sample, determines the Y axis coordinate Y of test sample datum markS；
Step 4: the method for the X-ray transmission intensity distribution irradiated using laser beam or penetrate sample datum mark using test is obtained
Take the Z axis coordinate Z of test sample datum markS；
Wherein, for single layer flat samples and hollow same wall thickness sample datum mark coordinate ZSAcquisition methods are as follows: by sample
Clamping keeps the surface normal at tested position parallel with X-ray incident direction on sample stage, is directed toward diffraction using X-direction
The laser of the round heart of instrument is positioned, and the Z axis coordinate Z of datum mark is obtainedS；
The hollow specimen datum mark Z axis coordinate acquiring method different for wall thickness are as follows: first one piece of thickness of clamping is equal on sample stage
Even plate sample (such as aluminium sheet), and make the planar surface normal parallel with X-ray incident direction, adjust the voltage of X-ray tube
And electric current, guarantee that x-ray photon counts the saturation count for being much smaller than detector when transmission；Then near 2 θ=0 °, 2 θ scanning
The curve that the x-ray count intensity of measurement transmission is distributed along 2 θ, carries out curve fitting, and calculates 2 angles θ for determining max transmissive intensity
Spend 2 θ of position0, and place the detector 2 θ0, that is, place the detector the angle position of face X source；Plate is removed again, in sample
The different hollow specimen of clamping wall thickness in sample platform, and make the surface normal at tested position parallel with X-ray incident direction, it adjusts
The voltage and current of whole X-ray tube, Z axis scanning survey transmission x-ray photon count intensity along coordinate Z distribution curve, into
The Smoothing fit of row curve finally combines known thickness of sample variation characteristic to choose the datum mark of test sample, determines test
The Z axis coordinate Z of sample datum markS；
Step 5: it is thick that test sample being obtained using the method that test penetrates the short wave length X-ray diffraction intensity distribution of sample datum mark
Spend the X axis coordinate X of directional reference pointS；
For single layer samples, step includes:
Step A: sample is first moved to coordinate YSAnd/or at coordinate Zs, X-axis is translated so that thickness of sample using ocular estimate
It is located at the round heart of diffractometer at center；Choose measurement short wavelength's characteristic X-ray WK α1Measure the diffraction of a certain hkl crystal face of sample
Spectrum；
Step B:2 θ (diffraction angle determines that d is interplanar distance from λ is X-ray wavelength according to Bragg's equation 2dsin θ=λ) step
Into short wavelength's characteristic X ray diffracting spectrum of the scanning survey crystal face, peak is determined to diffraction spectra, determines the angle of diffraction 2 of the hkl crystal face
θhkl；Fixed 2 θ of the angle of diffraction is placed the detector againhkl, the x-ray photon meter of X-axis translation scan measurement X axis coordinate X- diffraction
The curve of number intensity, carries out curve Smoothing fit, determines peak, obtain the X-coordinate x1 of diffracted intensity maximum value；
Step C: at sample coordinate X=x1, step-scan measures diffraction spectra, determines peak using parabolic method etc., fixed 2 θhkl' again will
Detector is placed in fixed 2 θ of the angle of diffractionhkl', X-axis translation scan measures the x-ray photon count intensity of X axis coordinate X- diffraction
Curve carries out curve Smoothing fit, determines peak, obtain the X-coordinate x1 ' of diffracted intensity maximum value；
Step D: the X axis coordinate X of test sample datum mark is determinedS.If | x1 ' |-| x1 | it is less than preset value, such as less than
0.01mm, it is believed that the X axis coordinate X of test sample datum markS=x1 '；Otherwise, step B, step C are repeated, until adjacent two
Until the secondary X-coordinate difference measured is less than preset value (such as less than 0.01mm), the X axis coordinate X of test sample datum markSFor
The X-coordinate for the diffracted intensity maximum value that last time measures；
For hollow specimen, step includes:
Step a: sample is first moved to coordinate YSAnd/or coordinate ZsPlace is translated X-axis so that hollow specimen using ocular estimate
It is located at the round heart of diffractometer at the mid-depth of side；Choose a certain hkl crystal face of a certain short wavelength's characteristic X-ray measurement sample
Diffraction spectra；
Step b:2 θ step-scan measures short wavelength's characteristic X ray diffracting spectrum of the hkl crystal face, determines peak to diffraction spectra, and determining should
2 θ of the angle of diffraction of hkl crystal facehkl；Fixed 2 θ of the angle of diffraction is placed the detector againhkl, X-axis translation scan measurement X axis coordinate X- spread out
The curve for the x-ray photon count intensity penetrated carries out curve Smoothing fit, determines peak, and two X for obtaining diffracted intensity maximum are sat
Mark x1, x2；
Step c: at sample coordinate X=x1, step-scan measures diffraction spectra, determines peak using parabolic method etc., fixed 2 θhkl' again will
Detector is placed in fixed 2 θ of the angle of diffractionhkl', X-axis translation scan measures the x-ray photon count intensity of X axis coordinate X- diffraction
Curve carries out curve Smoothing fit, determines peak, obtain two X-coordinate x1 ', x2 ' of diffracted intensity maximum；
Step d: if | x1 ' |-| x1 | and | x2 ' |-| x2 | it is less than preset value, such as less than 0.01mm, it is believed that test specimens
The X axis coordinate X of product datum markS=x1 ' or XS=x2 '；Otherwise, step b, step c are repeated, until the adjacent X measured twice is sat
Until mark difference is less than preset value (such as less than 0.01mm), the X axis coordinate X of test sample datum markSIt can be last
One of the X-coordinate of secondary two measured diffracted intensity maximum；
Step 6: according to the test sample datum mark coordinate X obtained in step 3,4 and 5S、YS、ZSWith the scale coordinate of test sample
Relationship calculates the three-dimensional coordinate for determining the other detected parts of test sample, true by the way that the X, Y, Z axis of sample stage is moved to calculating
At fixed detected part coordinate, so that test sample detected part to be positioned to the center of circle of short wave length X-ray diffraction instrument circle.
Attenuation by absorption and crystal diffraction method the present invention is based on sample to X-ray, by single layer flat samples, hollow
Same wall thickness sample, the samples datum mark such as the different hollow specimen of wall thickness measurement and positioning, it is real in conjunction with known sample structure
The accurate positioning to sample test position is showed.
The present invention, can not only be by interiors of products test position by the mutual cooperation of transmission detection and diffraction detection method
It is precisely positioned at the center of circle of X-ray diffractometer circle, and can accurately obtain the coordinate of any test position of interiors of products,
Especially suitable for the accurate positioning at hollow products close beta position, non-destructive testing, to analyze test sample internal stress, knit
Structure and object are equal.
Positioning method accuracy of the present invention is high, it can be ensured that the accuracy of detection, it can be by hollow products close beta position
Error of coordinate control within 0.05mm, successive ignition positioning or even can control error of coordinate as within 0.005mm；This
Any direction at ground non-destructive testing Centimeter Level thickness common used material and the surveyed position of workpiece can be accurately positioned in the method for invention
Stress can be applied to enterprise, research institution and colleges and universities, help accurately to analyze metal product, aerospace hollow component
Internal stress, texture, object phase, atomic distance etc..
Detailed description of the invention
Fig. 1 is the optical path and laser positioning schematic diagram of short wave length X-ray diffraction instrument of the present invention, incident X-rays X-axis just
Direction, negative direction of the direction that laser beam projects in X-axis；
In Fig. 1: 1.-heavy metal target X-ray tube, 2.-incidence collimator, the round heart of 3.-diffractometer, 4.-sample are clamped in sample
Platform 9. on, 5.-receive collimator, 6.-detector, 7.-X-direction laser, 8.-diffractometer circle, 9.-three-dimensional sample platform, 10.-
The X-ray of transmission,The X-ray of diffraction；Wherein: the vertical paper of the plane that Z axis is constituted perpendicular to XY axis is outside；
Fig. 2 is the solid sample schematic diagram of single layer plate in the embodiment of the present invention 1；
Fig. 3 is the Diffraction intensity distribution figure of single layer flat samples through-thickness X-coordinate in Fig. 2；
Fig. 4 is the identical hollow Ti Alloy Curved sample schematic diagram of wall thickness in the embodiment of the present invention 2；
Fig. 5 is the Diffraction intensity distribution figure of Ti Alloy Curved sample transversely X-coordinate in Fig. 4；
Fig. 6 is the intensity in transmission distribution map of wall thickness is different in the embodiment of the present invention 3 hollow titanium alloy sample transversely Y coordinate.
Specific embodiment
The present invention is further explained in the light of specific embodiments, it is pointed out here that following embodiment should not be understood as pair
The limitation of the scope of the present invention, those of ordinary skill in the art's content according to the present invention make it is some it is nonessential improvement and
Adjustment, all falls in the scope of protection of the present invention.Equipment used in the embodiment of the present invention is shortwave disclosed in CN100485373C
Long X-ray diffraction measurement device.
Embodiment 1
As shown in Fig. 2, institute's sample is the fine grain sheet metal of 20mm*20mm*0.5mm, short wave length X-ray diffraction is set
The threshold up and down of the X-ray detection analysis system of instrument and use wavelength for the WK α of 0.0209nm1Measure diffracted intensity and diffraction
Spectrum, pipe press 200kv, and pipe stream 8mA, incident collimator and the angle of divergence for receiving collimator are 0.11 °, utilize laser positioning benchmark
The Y axis coordinate and Z axis coordinate of point, utilize the short wave length X-ray diffraction count intensity through-thickness of X-axis scanning survey transmission
Distribution, is accurately positioned the X axis coordinate of datum mark, specific as follows:
Step 1: the clamping sample on sample stage, so that being chosen as surface normal and the X-ray incidence of the test position of datum mark
Direction is parallel, utilizes the Ys=76.5mm of the laser positioning of the X-direction test position, Zs=32.4mm.It is directed toward diffractometer circle
The laser designation error in the center of circle is ± 0.05mm in Y-axis and Z axis error, meets required precision.X-axis is put down using ocular estimate
It moves so that being located at the round heart of diffractometer at the center of thickness of sample；
Step 2: choosing WK α1, 0.01 ° of 2 θ step-length, every step time of measuring 10s, step-scan measures spreading out for α-Fe (110) crystal face
Spectrum is penetrated, peak is determined using parabolic method etc., fixed 2 θ110=5.907 °；Place the detector 2 θ of the angle of diffraction110=5.907 °, setting X is swept
Measurement parameter is retouched, X step-length 0.5mm, every step time of measuring 10s are scanned measurement along X axis coordinate, determine peak, obtain diffracted intensity
Maximum X-coordinate X=-12.216mm；
Step 3: sample being moved at X=-12.21mm, diffraction spectra scanning survey parameter, 2 0.01 ° of θ step-lengths, every pacing are set
Time 10s is measured, step-scan measures diffraction spectra, determines peak using parabolic method etc., fixed 2 θ110=5.911 °.It places the detector and spreads out
2 θ of firing angle110=5.911 °, it is scanned measurement along X axis coordinate, the Diffraction intensity distribution along X-axis measured is as shown in figure 3, spread out
It penetrates spectrum smoothing fitting and determines peak, obtain the maximum X-coordinate X=-12.209mm of diffracted intensity；
Step 4: the X-coordinate facial difference 0.007mm < 0.01mm with last time, it is believed that the X-coordinate Xs of sheet metal mid-depth
=-12.209mm；
If calculating obtained X-coordinate differs larger with the coordinate X=-12.21mm of last time measuring and calculating, repeatedly walked in the present embodiment
Rapid 2, step 3, step 4, until difference is less than admitted value (such as 0.02mm or 0.005mm)；
Step 5: according to datum mark coordinate Xs=-12.209mm, Ys=76.5mm, the Zs=32.4mm of above-mentioned determination, control should
The scale coordinate relationship of flat samples drawing or flat samples calculates the three-dimensional coordinate for determining the other detected parts of flat samples,
It is calculated at determining detected part coordinate by moving to the X, Y, Z axis of sample stage to position flat samples detected part
In the center of circle of short wave length X-ray diffraction instrument circle.
Embodiment 2
As shown in figure 4, institute's sample is the titanium alloy bilayer curve hollow sample of 2mm wall thickness, setting short wave length X-ray spreads out
The WK α for penetrating the threshold up and down of the X-ray detection analysis system of instrument and using wavelength as 0.0209nm1Measure diffracted intensity and diffraction
Spectrum, pipe press 200kv, and pipe stream 4mA, incident collimator and the angle of divergence for receiving collimator are 0.11 °, utilize laser positioning benchmark
The Y axis coordinate and Z axis coordinate of point, utilize the short wave length X-ray diffraction count intensity through-thickness of X-axis scanning survey transmission
Distribution, is accurately positioned the X axis coordinate of datum mark, specific as follows:
Step 1: the clamping sample on sample stage, so that being chosen as surface normal and the X-ray incidence of the test position of datum mark
Direction is parallel, utilizes the Ys=112.7mm of the laser positioning of the X-direction test position, Zs=47.3mm.It is directed toward diffractometer circle
The laser designation error in the center of circle is ± 0.05mm in Y-axis and Z axis error, meets required precision；
Step 2: choosing α-Ti (002) crystal face as diffraction crystal face, place the detector 2 θ of the angle of diffraction002=5.117 °, X is set
Scanning survey parameter, X step-length 0.3mm, every step time of measuring 60s are scanned measurement along X axis coordinate, it is strong two diffraction occur
Maximum is spent, as shown in Figure 5.Smoothly determine peak, obtain the maximum X-coordinate of diffracted intensity be X=-29.478mm respectively with-
20.895mm；
Step 3: sample being moved at X=-20.895mm, diffraction spectra scanning survey parameter, 2 0.01 ° of θ step-lengths, every step are set
Time of measuring 60s, step-scan measure diffraction spectra, determine peak using parabolic method etc., fixed 2 θ002=5.113 °；
Step 4: placing the detector 2 θ of the angle of diffraction002=5.113 °, measurement, diffraction spectra Smoothing fit are scanned along X axis coordinate
Determine peak, obtain the maximum X-coordinate X=-20.882mm of diffracted intensity, the X-coordinate facial difference 0.013mm < 0.02mm with last time,
It is considered that the X-coordinate Xs=-20.882mm of the Ti Alloy Curved layer mid-depth close to detector side.If the X that this time obtains
Coordinate differs larger with coordinate X=-20.895mm, then repeatedly step 3, step 4 in the present embodiment, until difference is less than admitted value
Until.Similarly, step 3, step 4 in the present embodiment are repeated, can be located remotely from the Ti Alloy Curved thickness degree of detector side
The X-coordinate of other test positions can be calculated by obtained Xs by heart coordinate Xs=-29.483mm；
Step 5: according to the datum mark coordinate Xs=- of the Ti Alloy Curved layer mid-depth of identified close detector side
20.902mm, Ys=112.7mm, Zs=47.3mm, the benchmark far from the Ti Alloy Curved layer mid-depth close to detector side
Point coordinate Xs=-29.483mm, Ys=112.7mm, Zs=47.3mm, compare the titanium alloy bilayer curve hollow of the 2mm wall thickness
Sample drawing or its scale coordinate relationship calculate the three-dimensional coordinate for determining the other detected parts of the sample, by by sample stage
X, Y, Z axis, which moves to calculate, spreads out at determining detected part coordinate to which the sample detected part is positioned at short wave length X-ray
Penetrate the center of circle of instrument circle.
Embodiment 3
As shown in fig. 6, institute's sample is the different hollow titanium alloy sample of wall thickness, side wall thickness is 1mm thick, another side wall
Thickness is up to 3mm, minimum 1mm thickness zigzag sample.The sample is sealing structure, it is difficult to directly observe its internal thickness feelings
Condition.The incident collimator of short wave length X-ray diffraction instrument and the angle of divergence for receiving collimator are 0.11 °, and the X for setting instrument is penetrated
The threshold up and down of line detecting analytic system and use wavelength for the WK α of 0.0209nm1When measuring diffracted intensity and diffraction spectra, pipe pressure
200kv, pipe stream 4mA utilize the Z axis coordinate of laser positioning sample datum mark；Vertical incidence sample is measured using direct Y axis scanning
Transmission X-ray intensity distribution, be accurately positioned sample datum mark Y axis coordinate；The short wavelength X transmitted using X-axis scanning survey
X ray diffraction counts the distribution of intensity through-thickness, is accurately positioned X axis coordinate, specific as follows:
Step 1: the thick uniform aluminium sheet of one piece of 10mm of clamping on sample stage, and make the surface of aluminum plate normal and X-ray incidence side
To parallel, the voltage and current of X-ray tube is adjusted, guarantees that x-ray photon counts the saturation count for being much smaller than detector when transmission；
In this step, aluminium plate thickness includes but is not limited to 10mm, and the purpose using aluminium sheet is to place the detector face X source
Angle position；
Step 2: near 2 θ=0 °, it is quasi- to carry out curve for the curve that the x-ray count intensity of 2 θ scanning surveys transmission is distributed along 2 θ
It closes, calculates 2 angle position θ, 2 θ for determining max transmissive intensity0, and place the detector 2 θ0, that is, place the detector face X-ray
The angle position in source；
Step 3: unloading lower aluminum sheet, the clamping sample on sample stage, so that being chosen as the surface normal and X of the test position of datum mark
Ray incident direction is parallel, is irradiated to using the Zs=23.1mm of the laser positioning of the X-direction test position, and as laser beam
The label of specimen surface positions.It is directed toward the laser designation error of the round heart of diffractometer, is ± 0.05mm in Z axis error, is met
Required precision；
Step 4: adjusting voltage=45kv of X-ray tube, electric current=2mA guarantees that x-ray photon is counted much smaller than detection when transmission
The Y-axis step scan of the saturation count of device, 0.5mm measures distribution curve of the x-ray photon count intensity along coordinate Y of transmission,
The Smoothing fit for carrying out curve chooses the benchmark of test sample in conjunction with known sample interior shape (i.e. the feature of thickness change)
Point determines the Y axis coordinate Y of test sample datum markS=101.21mm；
Step 5:, to the identical method of step 4, determining the X axis coordinate X of test sample datum mark using with step 2 in embodiment 2S
=7.723mm；
Step 6: according to datum mark coordinate Xs=7.723mm, Ys=101.21mm, the Zs=23.1mm of above-mentioned determination, control should
Hollow titanium alloy sample drawing or its scale coordinate relationship calculate the three-dimensional coordinate for determining the other detected parts of the sample, pass through
The X, Y, Z axis of sample stage is moved to and is calculated at determining detected part coordinate to which the sample detected part is positioned at shortwave
The center of circle of long X-ray diffractometer circle.
Claims (4)
1. a kind of localization method of short wave length X-ray diffraction test sample, it is characterised in that steps are as follows:
Step 1: test sample being fixedly installed on the sample stage of short wave length X-ray diffraction device；
Step 2: choosing a certain test position of test sample as datum mark；
Step 3: the method for the X-ray transmission intensity distribution irradiated using laser beam or penetrate sample datum mark using test is obtained
Take the Y axis coordinate Y of test sample datum markS；
Step 4: the method for the X-ray transmission intensity distribution irradiated using laser beam or penetrate sample datum mark using test is obtained
Take the Z axis coordinate Z of test sample datum markS；
Step 5: it is thick that test sample being obtained using the method that test penetrates the short wave length X-ray diffraction intensity distribution of sample datum mark
Spend the X axis coordinate X of directional reference pointS；
Step 6: according to the test sample datum mark coordinate X obtained in step 3,4 and 5S、YS、ZSWith the scale coordinate of test sample
Relationship calculates the three-dimensional coordinate for determining the other detected parts of test sample, true by the way that the X, Y, Z axis of sample stage is moved to calculating
At fixed detected part coordinate, so that test sample detected part to be positioned to the center of circle of short wave length X-ray diffraction instrument circle.
2. the localization method of short wave length X-ray diffraction test sample as described in claim 1, it is characterised in that:
The coordinate Y of test sample datum mark is obtained using laser beam irradiation or X-ray transmission test sampleS、ZSStep includes:
For single layer samples and hollow same wall thickness sample datum mark Y-axis, Z axis coordinate acquiring method are as follows: by sample clamping
On sample stage, keep the surface normal at tested position parallel with X-ray incident direction, diffractometer circle is directed toward using X-direction
The laser in the center of circle is positioned, and the Y axis coordinate Y of datum mark is obtainedS, Z axis coordinate ZS；
The hollow specimen datum mark Y-axis different for wall thickness, Z axis coordinate acquiring method are as follows: first one piece of thickness of clamping on sample stage
Uniform plate is spent, and makes the planar surface normal parallel with X-ray incident direction, adjusts the voltage and current of X-ray tube,
Guarantee that x-ray photon counts the saturation count for being much smaller than detector when transmission, then in the X of 2 θ=0 ° scanning survey transmission nearby
The curve that ray count intensity is distributed along 2 θ, carries out curve fitting, and calculates 2 angle position θ, 2 θ for determining max transmissive intensity0,
And place the detector 2 θ0；Plate is removed again, the different hollow specimen of clamping wall thickness on sample stage, and make tested portion
The surface normal of position is parallel with X-ray incident direction；The voltage and current of X-ray tube is adjusted, the X of Y axis scanning measurement transmission is penetrated
Linear light sub-count intensity carries out the Smoothing fit of curve along the distribution curve of coordinate Y, according to the variation of distribution curve, in conjunction with
The datum mark for the thickness change Feature Selection test sample known determines the Y axis coordinate Y of test sample datum markS；The sample is existed
Y-axis moves to YSPlace, the x-ray photon count intensity of Z axis scanning survey transmission carry out curve along the distribution curve of coordinate Z
Smoothing fit is determined and is surveyed in conjunction with the datum mark of known thickness change Feature Selection test sample according to the variation of distribution curve
The Z axis coordinate Z of test agent datum markS。
3. the localization method of short wave length X-ray diffraction test sample as claimed in claim 2, it is characterised in that:
For single layer samples, is obtained and surveyed using the method that test penetrates the short wave length X-ray diffraction intensity distribution of sample datum mark
The X axis coordinate X of test agent thickness direction datum markSStep includes:
Step A: sample is first moved to coordinate YSAnd/or at coordinate Zs, X-axis is translated so that thickness of sample using ocular estimate
It is located at the round heart of diffractometer at center, chooses the diffraction spectra of a certain hkl crystal face of a certain short wavelength's characteristic X-ray measurement sample；
Step B:2 θ step-scan measures short wavelength's characteristic X ray diffracting spectrum of the hkl crystal face, determines peak to diffraction spectra, and determining should
2 θ of the angle of diffraction of hkl crystal facehkl；Fixed 2 θ of the angle of diffraction is placed the detector againhkl, X-axis translation scan measurement X axis coordinate X- spread out
The curve for the x-ray photon count intensity penetrated carries out curve Smoothing fit, determines peak, obtain the X-coordinate of diffracted intensity maximum value
x1；
Step C: at sample coordinate X=x1, step-scan measures diffraction spectra, using the legal peak of parabola, fixed 2 θhkl' will visit again
It surveys device and is placed in fixed 2 θ of the angle of diffractionhkl', X-axis translation scan measures the song of the x-ray photon count intensity of X axis coordinate X- diffraction
Line carries out curve Smoothing fit, determines peak, obtain the X-coordinate x1 ' of diffracted intensity maximum value；
Step D: if | x1 ' |-| x1 | it is less than preset value, it is believed that the X axis coordinate X of test sample datum markS=x1 '；It is no
Then, step B, step C are repeated, until the adjacent X-coordinate difference measured twice is less than preset value, test sample benchmark
The X axis coordinate X of pointSFor the X-coordinate of the diffracted intensity maximum value measured for the last time.
4. the localization method of short wave length X-ray diffraction test sample as claimed in claim 2, it is characterised in that:
For hollow specimen, is obtained and surveyed using the method that test penetrates the short wave length X-ray diffraction intensity distribution of sample datum mark
The X axis coordinate X of test agent thickness direction datum markSStep includes:
Step a: sample is first moved to coordinate YSAnd/or at coordinate Zs, X-axis is translated so that hollow specimen using ocular estimate
It is located at the round heart of diffractometer at the mid-depth of side, chooses a certain hkl crystal face of a certain short wavelength's characteristic X-ray measurement sample
Diffraction spectra；
Step b:2 θ step-scan measures short wavelength's characteristic X ray diffracting spectrum of the hkl crystal face, determines peak to diffraction spectra, and determining should
2 θ of the angle of diffraction of hkl crystal facehkl；Fixed 2 θ of the angle of diffraction is placed the detector againhkl, X-axis translation scan measurement X axis coordinate X- spread out
The curve for the x-ray photon count intensity penetrated carries out curve Smoothing fit, determines peak, and two X for obtaining diffracted intensity maximum are sat
Mark x1, x2；
Step c: at sample coordinate X=x1, step-scan measures diffraction spectra, using the legal peak of parabola, fixed 2 θhkl' will visit again
It surveys device and is placed in fixed 2 θ of the angle of diffractionhkl', X-axis translation scan measures the song of the x-ray photon count intensity of X axis coordinate X- diffraction
Line carries out curve Smoothing fit, determines peak, obtain two X-coordinate x1 ', x2 ' of diffracted intensity maximum；
Step d: if | x1 ' |-| x1 | and | x2 ' |-| x2 | it is less than preset value, it is believed that the X-axis of test sample datum mark
Coordinate XS=x1 ' or XS=x2 '；Otherwise, step b, step c are repeated, until the adjacent X-coordinate difference measured twice is less than in advance
Until first setting value, the X axis coordinate X of test sample datum markSIt is sat for the X of the two diffracted intensity maximum measured for the last time
One of mark.
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