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CN108613641A - Two-dimentional orientation error precision measurement method for thin plate crystals - Google Patents

Two-dimentional orientation error precision measurement method for thin plate crystals Download PDF

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Publication number
CN108613641A
CN108613641A CN201810813573.4A CN201810813573A CN108613641A CN 108613641 A CN108613641 A CN 108613641A CN 201810813573 A CN201810813573 A CN 201810813573A CN 108613641 A CN108613641 A CN 108613641A
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measured
crystal
directions
orientation error
angles
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CN108613641B (en
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安宁
吴华峰
李朝阳
徐勇
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Anhui Specreation Instrument Science & Technology Co ltd
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Anhui Chuang Pu Instrument Technology Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B15/00Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/20Investigating 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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  • Chemical & Material Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
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Abstract

The invention discloses a kind of two-dimentional orientation error precision measurement methods for thin plate crystals, crystal prototype to be measured is fixed on suction disc in method, detector is rotated with X ray angles to 2 times of the angles Bragg, crystal prototype to be measured is scanned around the angles θ in the directions z using precise rotating platform, the phase angle of crystal prototype to be measured is rotated around the directions y and is changedUntil 360 ° of rotations are completed at the phase angle of crystal prototype to be measured.Two-dimentional orientation error may be implemented using the above method to measure;Standard crystal is not depended on, measurement result precision is high;It can obtain two aspect information of orientation error size and direction.

Description

Two-dimentional orientation error precision measurement method for thin plate crystals
Technical field
The present invention relates to a kind of crystal orientation error measuring system and measurement methods, more particularly to one kind to be spread out based on X-ray Technology is penetrated, the two-dimentional accurate measurement of thin plate crystals orientation error is suitable for, belongs to crystal X-ray detection the relevant technologies.
Background technology
Crystal is a kind of material being widely used in semi-conductor industry and X-ray light splitting field.In crystallography, pass through Crystal face is defined the arrangement orientation of crystals atom is described.To different use occasions and crystalline, need to select Different crystal faces.However, in actual production process, there may be angles between selected crystal face and crystallophy surface.
Orientation error is defined as the angle between crystal face normal direction and physical surface normal direction.The presence of orientation error can be to crystal Performance has various influences:In semiconductor industry, orientation error can cause the electricity of crystal, magnetic property to change Become, influences electronic component performance.In X-ray optical field, orientation error can influence crystal photoelement energy and space point Resolution.Therefore, the orientation error for accurately measuring crystal is of great significance.In order to accurately measure orientation error, measures content and answer Including three aspects:1. the size of orientation error;2. the direction of orientation error;3. the Two dimensional Distribution of orientation error.Only by this Three parameters are all measured, and could describe the orientation error of crystal perfectly.
Currently, X-ray diffraction (X-ray diffraction, abbreviation XRD) is a kind of common crystal detection means.Root According to Bragg principles, X-ray wavelength has following relationship with crystal interplanar distance and the angles Bragg:
N λ=2d sin θs are 1.
Wherein, n is diffraction time, and λ is X-ray wavelength, and d is spacing of lattice, and θ is the angles Bragg.Therefore, when monochromatic X- is penetrated When line is radiated on crystal face, the light of certain degree is only formed with crystal face can just occur diffraction, this is the base of XRD crystal detection Plinth.
When existing crystal direction finder is by measuring monochromatic x-rays by crystal diffraction, crystallophy surface and incident light Angle, and using the difference at the angle and the angles Bragg as the orientation error of crystal.But this measurement method has three aspects to ask Topic:
1. the X-ray hot spot being radiated on crystal is larger, the orientation error measured is being averaged in entire spot area Value, sample stage also do not have translation functions, are unable to get the Two dimensional Distribution of orientation error;
2. the orientation error measured is projection of the actual orientation error in the direction, measurement result is inaccurate, meanwhile, it is existing The direction of orientation error can not be measured by having equipment also;
3. the angle of sample stage needs benchmark, existing method be demarcated using standard crystal, then, standard crystal sheet The orientation error of body will accumulate in final measurement result.
As it can be seen that existing direction finder cannot be satisfied the demand of two-dimension high-precision crystal orientation.
Invention content
The object of the present invention is to provide a kind of two-dimentional orientation errors to thin plate crystals to implement accurate measure.
A kind of two-dimentional orientation error precision measurement method of thin plate crystals, includes the following steps:
Step 1:It is zero or initial bit by the playback of index table, precise rotating platform and two-dimension translational platform, crystal prototype to be measured is solid It is scheduled on suction disc;
Step 2:The measuring point on theoretical interplanar distance, the directions x and the directions z of crystal prototype to be measured is inputted in the controls The angle interval that spacing and measuring point quantity, azimuth rotate every time
Step 3:Control system is managed according to the theoretical interplanar distance inputted in monochromatic x-rays wavelength, above-mentioned steps 2 The angles Bragg of opinion, control precise rotating platform rotate the plane of crystal to be measured of crystal prototype to be measured and X-ray angle to Bragg Angle, and detector and X-ray angle are rotated to 2 times of the angles Bragg;
Step 4:Crystal prototype to be measured is scanned around the angles θ in the directions z using precise rotating platform, when detector signal reaches It is most strong, by angular encoder record around the corner numerical value in the directions z;
Step 5:It controls index table and rotates at the phase angle of crystal prototype to be measured around the directions y and changeRepeat step 4;
Step 6:Step 5 is repeated, completing 360 ° until the phase angle of crystal prototype to be measured rotates, that is, completes the survey of the position Amount;
Step 7:According to the measuring point spacing and measuring point quantity on the directions x and the directions z, control two-dimension translational platform moves crystalline substance to be measured Body sample is to next measurement position;
Step 8:Step 4~7 are repeated, until completing the measurement to all positions on crystal prototype to be measured;
Step 9:It is carried out accordingly to each measurement position phase angle and around the directions z corner numerical value using following relationship Fitting, you can obtain the Two dimensional Distribution of crystal prototype orientation error to be measured:
In above-mentioned relation formula, Δ θ is θ variable quantities, characterizes the reading that sample stage is rotated around z-axis, is the data measured;α For the size of orientation error, it is the projection of surface normal rotational trajectory circle in the x direction to characterize brilliant Δ θ to be measured.
Using above-mentioned measurement method, technique effect is embodied in following several respects:1. two-dimentional orientation error may be implemented to measure; 2. not depending on standard crystal, measurement result precision is high;3. two aspect information of orientation error size and direction can be obtained.
Description of the drawings
Fig. 1 is the measuring principle schematic diagram of the present invention;
Fig. 2 is the definition schematic diagram of relevant parameter;
Fig. 3 is the structural schematic diagram of the present invention.
Specific implementation mode
Embodiment 1
The present embodiment is exactly test method and the description that is carried out in advance to system for convenience of description.In conjunction with Fig. 3, it is used for The two-dimentional orientation error precision measurement system of thin plate crystals, X-ray source 20, X-ray source 20 obtain after exposing to monochromator 30 Monochromatic light directed crystal prototype A to be measured is provided with holder on workbench 10 and fixes crystal prototype A to be measured, and holder is around positioned at vertical The Z axis in direction is vertically positioned in the rotation of horizontal direction Y-axis with Z axis, and holder straight-line displacement on the direction perpendicular to Y-axis is to be measured The crystal face to be measured of crystal prototype A is vertical with Y-axis.
The X-ray sent out by X-ray source 20 forms monochromatic light by monochromator 30, and passes through collimation diaphragm 40, purpose It is to obtain the monochromatic x-rays of small size small divergence angle, realizes the measurement to the parts crystal prototype A to be measured.It in this way can be to avoid survey The excessive caused average effect in region is measured, measurement accuracy and spatial discrimination are improved.
Crystal prototype A to be measured is mounted on workbench 10, it is desirable that meeting basic function includes:(1) fixes crystalloids to be measured Product A;(2) realizes Bragg angle precision sweeps, is rotated in Fig. 1 around the directions z;(3) angle recordings;(4) realizes azimuth rotation Turn, is rotated around the directions y in Fig. 1;(5) realizes two-dimensional movement, the directions x and the translation of the directions z in Fig. 1.The implementation of certain above-mentioned movement Posture and the position of crystal prototype A to be measured are mainly adjusted, these rotations or movement realize have below by relevant mechanism Body explanation.
Holder includes sucker or plate 51, attaching side plate face with the back side of crystal prototype A to be measured and be laid on suction disc 51 The sucker being connected with vacuum environment, suction disc 51 are connected on the dynamic platform 52 of index table 50, are moved platform 52 and are rotated around Y-axis.Crystalline substance to be measured The fixed form of body sample A can be mechanical or air suction type etc., it is desirable that fix thin plate crystals smooth.
The Jing Tai of index table 50 is connected on the dynamic pedestal 61 of precise rotating platform 60, moves Z axis of the pedestal 61 around vertical direction Rotation.
Precise rotating platform 60 is the angles Bragg precision sweep device, and effect is the precision for realizing crystal prototype A to be measured around the directions z Scanning changes angle, the i.e. angles Bragg between X-ray and crystal face.The effect of angle recordings is crystalline substance to be measured during record measures every time Variable quantity of the body around the precision sweep of the directions z.Index table 50 is to realize azimuth rotary setting, and effect is to realize crystal around y The rotation in direction, is rotated by azimuth, can be completed measurement of the crystal under different orientations, is somebody's turn to do by data processing The orientation error of position crystal.
Collimation diaphragm 40 is set between monochromator 20 and the crystal face to be measured of crystal prototype A to be measured, and crystal prototype A's to be measured waits for It surveys and arranges detector 70 on the reflection direction of the reflected light of crystal face.The arrangement of this incident light can be to avoid measured zone mistake Big caused average effect.
The two-dimension translational platform 80 that guide and limit mechanism is constituted is set between suction disc 51 and dynamic platform 52, and two-dimension translational platform 80 includes Orthogonal in-plane displancement guiding mechanism, the displacement surface are vertical with Y direction.
The effect of two-dimensional movement is the movement for realizing the crystal face to be measured of crystal prototype A to be measured in xOz planes, reaches measurement The purpose of two-dimentional orientation error.
The present invention measuring system require precise rotating platform 60 be the angles Bragg precision sweep shaft, that is, Fig. 1 in the directions z, point Degree turntable 50 is that the directions y in azimuth rotating shaft, that is, Fig. 1 are intersected with X-ray optical axis;Also, the intersection point is located at crystalline substance to be measured Body surface face.On the one hand it can ensure that X-ray is radiated at plane of crystal to be measured always when carrying out Bragg angle precision sweeps in this way Same position, on the other hand can ensure that X-ray is radiated at crystal table to be measured always when changing crystal orientation angle to be measured The same position in face.
The measuring system of the present invention require the physical surface of crystal to be measured with index table 50 i.e. azimuth rotating shaft i.e. The directions y in Fig. 1 are vertical, can ensure the angle i.e. crystal face normal direction of measured crystal face normal direction and azimuth rotating shaft in this way With the angle of physical surface normal direction, that is, orientation error.
When O point of the x-ray irradiation of monochromatic small light spot on plane of crystal to be measured, only pressed from both sides in X-ray and crystal face When angle meets Bragg principles, monochromatic x-rays just can be by crystal diffraction.Realize crystal to be measured around z by workbench in the present invention The scanning of direction rotation.In scanning process, using the variation of X-ray intensity on 70 detection of diffracted direction of detector, work as intensity Reach maximum value, illustrates that the angle of X-ray at this time and crystal face is the angles Bragg θB, it is Δ that sample rotates corresponding reading around z-axis θ0.The statement connotation having the same of crystal to be measured and crystal prototype A to be measured.
Embodiment 2
A kind of two-dimentional orientation error precision measurement method of thin plate crystals, includes the following steps:
Step 1:It is zero or initial bit by the playback of index table 50, precise rotating platform 60 and two-dimension translational platform 80, crystal to be measured Sample A is fixed on suction disc 51;
Step 2:The survey on theoretical interplanar distance, the directions x and the directions z of crystal prototype A to be measured is inputted in the controls The angle interval that point spacing and measuring point quantity, azimuth rotate every time
Step 3:Control system is managed according to the theoretical interplanar distance inputted in monochromatic x-rays wavelength, above-mentioned steps 2 The angles Bragg of opinion, control precise rotating platform 60 by the plane of crystal to be measured of crystal prototype A to be measured and X-ray angle rotate to The angles Bragg, and detector 70 and X-ray angle are rotated to 2 times of the angles Bragg;Step 4:Using precise rotating platform 60 to be measured Crystal prototype A is scanned around the angles θ in the directions z, when 70 signal of detector reaches most strong, is recorded around the side z by angular encoder To corner numerical value;
Step 5:It controls index table 50 and rotates at the phase angle of crystal prototype A to be measured around the directions y and changeIt repeats Step 4;
Step 6:Step 5 is repeated, completing 360 ° until the phase angle of crystal prototype A to be measured rotates, that is, completes the position It measures;
Step 7:According to the measuring point spacing and measuring point quantity on the directions x and the directions z, control two-dimension translational platform moves crystalline substance to be measured Body sample A is to next measurement position;
Step 8:Step 4~7 are repeated, until completing the measurement to all positions on crystal prototype A to be measured;
Step 9:It is carried out accordingly to each measurement position phase angle and around the directions z corner numerical value using following relationship Fitting, you can obtain the Two dimensional Distribution of crystal prototype A orientation errors to be measured:
In above-mentioned relation formula, Δ θ is θ variable quantities, characterizes the reading that sample stage is rotated around z-axis, is the data measured;α For the size of orientation error, it is the projection of surface normal rotational trajectory circle in the x direction to characterize brilliant Δ θ to be measured.
Sample stage is rotated by a certain angle around the directions y, that is, changes the azimuth of crystal to be measuredDue to azimuth shaft (directions y) intersects at O points with X-ray, then, X-ray is still radiated on O points after rotation.But due to orientation error The angle of the presence of α, X-ray and crystal face can change, and cause X-ray can not be by crystal diffraction.At this point, passing through sample again Platform carries out angle scanning of the crystal to be measured around the directions z, when the signal strength that detector detects reaches maximum value, sample stage again It is Δ θ to rotate corresponding reading around the directions z1.Successively by Crystal Rotation to be measured to different orientations, and measure Δ θi
Since azimuth shaft and plane of crystal normal direction are parallel, if being reference with crystal face normal direction, in circular dividing table 50 In rotary course, it is equivalent to surface normal direction and is rotated around normal of crystal surface direction.On the other hand, each Δ θ is in X-ray Angle with crystal face is θBWhen obtain, so measuring principle can be reduced to Fig. 2, i.e.,:In measurement process, surface normal phase Crystal face normal direction is rotated, in order to make θBSize remains unchanged, and needs the size for changing θ.The variation delta θ of θ by orientation error α and Rotation phaseIt codetermines.As shown in Fig. 2, Δ θ is the projection of surface normal rotational trajectory circle in the x direction, meet such as ShiShimonoseki System:
As shown in Fig. 2, relational expression 2. in, Δ θ be θ variable quantities, characterize the reading that sample stage rotate around z-axis, be survey The data obtained;α is the size of orientation error, characterizes the angle between crystal crystal face normal direction and physical surface normal direction to be measured, Φ is The phase of orientation error, when to be characterized in azimuth be 0, in the angle of xOz plane projections and x positive directions, the two is orientation error It is to be measured;It is azimuth, the angle rotated around y-axis by sample stage provides;ω is orientation ascent, since Δ θ periods of change are Therefore 2 π work as azimuthWhen using radian as unit, ω=1, whenWhen using angle as unit, ω=π/180;θBFor Bragg Angle is obtained by theoretical calculation.
By data (Δθ0)、(Δθ1)、(Δθ2)、……(Δθn) be 2. fitted according to relational expression, you can To the orientation error information of O points.

Claims (1)

1. a kind of two-dimentional orientation error precision measurement method of thin plate crystals, includes the following steps:
Step 1:It is zero or initial bit by the playback of index table (50), precise rotating platform (60) and two-dimension translational platform (80), crystalline substance to be measured Body sample (A) is fixed on suction disc (51);
Step 2:The measuring point on theoretical interplanar distance, the directions x and the directions z of crystal prototype to be measured (A) is inputted in the controls The angle interval that spacing and measuring point quantity, azimuth rotate every time
Step 3:Control system obtains theory according to the theoretical interplanar distance inputted in monochromatic x-rays wavelength, above-mentioned steps 2 The angles Bragg, control precise rotating platform (60) by the plane of crystal to be measured of crystal prototype to be measured (A) and X-ray angle rotate to The angles Bragg, and detector (70) and X-ray angle are rotated to 2 times of the angles Bragg;
Step 4:Crystal prototype to be measured (A) is scanned around the angles θ in the directions z using precise rotating platform (60), when detector (70) Signal reaches most strong, by angular encoder record around the corner numerical value in the directions z;
Step 5:It controls index table (50) and rotates at the phase angle of crystal prototype to be measured (A) around the directions y and changeIt repeats to walk Rapid 4;
Step 6:Step 5 is repeated, completing 360 ° until the phase angle of crystal prototype to be measured (A) rotates, that is, completes the survey of the position Amount;
Step 7:According to the measuring point spacing and measuring point quantity on the directions x and the directions z, control two-dimension translational platform moves crystalloids to be measured Product (A) extremely next measurement position;
Step 8:Step 4~7 are repeated, until completing the measurement to all positions on crystal prototype to be measured (A);
Step 9:Using following relationship is to each measurement position phase angle and around the directions z, corner numerical value is intended accordingly It closes, you can obtain the Two dimensional Distribution of crystal prototype to be measured (A) orientation error:
In above-mentioned relation formula, Δ θ is θ variable quantities, characterizes the reading that sample stage is rotated around z-axis, is the data measured;α is fixed To the size of error, it is the projection of surface normal rotational trajectory circle in the x direction to characterize brilliant Δ θ to be measured.
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CN113427650B (en) * 2021-06-17 2023-03-14 西北工业大学 Method for measuring orientation of directionally solidified alloy single crystal and cutting seed crystal

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