CN100504349C - X ray diffraction instrument and method for detecting macro stress in micro area - Google Patents
X ray diffraction instrument and method for detecting macro stress in micro area Download PDFInfo
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- CN100504349C CN100504349C CNB2007100552098A CN200710055209A CN100504349C CN 100504349 C CN100504349 C CN 100504349C CN B2007100552098 A CNB2007100552098 A CN B2007100552098A CN 200710055209 A CN200710055209 A CN 200710055209A CN 100504349 C CN100504349 C CN 100504349C
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Abstract
A method of using X-ray diffraction device to detect macropress of micro-domain includes regulating surface of detected sample on rotary detection table to be vertical to round platform of X-ray diffractometer, setting heel shaft on cross line of said round platform with sample surface, selecting stress detection point under microscope, setting stress detection direction through rotary angle and confirming heel angle, measuring selected diffraction crystal surface under microscope to obtain relevant data then calculating out macropress value at vertical direction of heel shaft in micro-domain.
Description
Technical field
The invention belongs to field tests, particularly the method for testing of the x line diffraction of macro-stress variable gradient on tiny area and macro-stress skewness.
Background technology
, air-sensitive film device photosensitive for semiconductor, extensive electronics integrated device and some miniature precision instrument parts, the unavoidable macro-stress that produces in manufacture process.The mechanical property that this macro-stress is not only damaged device also produces very important influence to the photoelectric characteristic of device.Therefore, it is very necessary to detect this macro-stress accurately.
The macro-stress x ray detection of present material is recommended on wide-angle x line diffractometer or the special-purpose x ray stress instrument usually carries out.Its detection method is seen " X ray stress determination method ", An Zhengzhi, the nineteen ninety P57 of publishing house of Wang Wen space Jilin University～183.
Because the x radiation exposure area (being the analyzing and testing zone) of this quasi-instrument is bigger, the minimum detection zone of for example special-purpose x ray stress detector is: 2mm * 3mm=6mm
2It is also bigger than the surface detected of above-mentioned thin-film device and precision instrument part under many circumstances, therefore be difficult to realize that effective macro-stress detects, more can't implement the analyzing and testing of STRESS VARIATION gradient and stress distribution unevenness certainly above-mentioned micro devices.And specialized equipment function singleness cost is also high.
Summary of the invention
The technical problem to be solved in the present invention is the technical barrier that overcomes in the background technology, select suitable commercially available diffractometer for use, for it prepares a kind of accessory, complementary fit by both makes this complete equipment produce new measuring ability, and this measuring ability is that current any commercially available x x ray diffractometer x is not available, thereby, can detect the macro-stress variable gradient and the stress distribution of tiny area.
The x ray diffraction device of detection tiny area macro-stress of the present invention comprises an x x ray diffractometer x, is equipped with the primary ray collimator that is less than or equal to Φ 0.1mm; The online viewing microscope of sample and sample plummer and laser ranging system with energy X, Y, three translation motions of Z.
The device that the present invention developed is a covering device that increases on the sample plummer---the rotation monitor station.
The rotation monitor station that on the sample plummer, is equipped with, as the table top of placing sample, table top side and trimming bolt mesh by the disk that has the rotation angle scale, and can make table top serves as that axle rotates and indicate rotation angle Φ with the Z direction; Diameter along table top is provided with the inclination rotating shaft, semicircle bevel protractor is housed on the Z direction, and the center of circle vertical with the inclination rotating shaft, the plane of bevel protractor is in the inclination rotating shaft, when table top angle footage number when the inclination rotating shaft is rotated illustrates side rake angle α, said side rake angle α is the angle of detected sample surfaces and diffraction disk.
During test, detected sample is placed on the middle section of rotation monitor station.
The effect of rotation monitor station is to guarantee that detected sample can rotate 360 ° of angles around Z-direction around X-direction half-twist angle.The precision of rotation monitor station rotary manipulation preferably is equal to or higher than 0.2 °.
The x x ray diffractometer x that the present invention is selected should be equipped with and is not more than
0.1mm the primary ray collimator, detect guarantee to realize tiny area stress; Be equipped with the online viewing microscope of sample, to guarantee on detected sample, the to choose stress check point intuitively; But sample plummer and laser ranging system with X, Y, three translations of Z so that the accuracy of measurement point set positions is not less than 0.01mm, and guarantee simultaneously the stress check point be arranged on accurately diffractometer diffraction circle in the heart.The D8C that Germany Brooker company produces
2Combinatorial chemistry x x ray diffractometer x is exactly an example that can satisfy in the commercially available equipment of above requirement.
The present invention adopts inclination method tiny area macro-stress detection method, uses the x x ray diffractometer x that is equipped with the rotation monitor station; The detection step has:
The 1 detected sample surfaces of adjusting on the rotation monitor station is vertical with x x ray diffractometer x diffraction circle platform, and the inclination rotating shaft is arranged on the intersection of diffraction disk and detected sample surfaces.
2 select stress check point O at microscopically.
3 by rotation angle Φ set the stress detection side to.
4 determine side rake angle α, and side rake angle α is detected sample surfaces and incident x ray I
0And the diffraction disk angulation of diffraction x ray I formation.
5 observe stress check point O again at microscopically, adjust check point O and justify the center with diffraction and overlap.
6 measure selected diffraction crystal face (hkl).
7 couples of selected stress check point O repeat 5 and 6 steps under different side rake angle α situations, obtain one group of 2 θ α data.
8 calculate in the O point tiny area on the detected sample with roll axis AB vertical direction on the macro-stress value.
In step 7, repeat 5 and 6 steps under the said different side rake angle α situations, side rake angle α can select α=0 °, α=16 °, α=24 °, α=30 ° to carry out duplicate measurements.
In step 8, said calculating can be calculated by the method that background technology " X ray stress determination method " provides.
New measuring ability of the present invention is: on gadget, can intuitive and accurately choose the stress check point, and (0.01mm near the tiny area check point
2～0.03mm
2) measurement of enforcement macro-stress; On gadget, be not less than the variable gradient that detects stress in the distance range of 1mm, be not less than 1mm
2Area of detection in observation stress distribution unevenness.Characteristics of the present invention in sum are:
The tiny area macro-stress detection method that 1 the present invention proposes can detect the macro-stress on the inherent assigned direction arbitrarily in zone of any appointment of detected sample.
2 this methods can be implemented macro-stress at tiny area to detected sample and detect.
3 this methods can detect the STRESS VARIATION gradient to detected sample in the distance range of 1mm～5mm.
4 this methods can be not less than 2mm to detected sample
2The zonule in detect the stress distribution unevenness.
5 this detection methods are by a selected commercially available x x ray diffractometer x and a home-made contrivance---rotate the monitor station realization that matches.
Description of drawings
Fig. 1 is a rotation monitor station principle schematic of the present invention.
Fig. 2 is the part weld metal zone macro-stress variable gradient curve that records with the inventive method.
Fig. 3 is the Probability Distribution figure that occurs with the diamond film stress that the inventive method records.
Embodiment
Home-made contrivance among embodiment 1 the present invention---the rotation monitor station that a kind of inclination method tiny area macro-stress detects.
See Fig. 1, selecting D8C for use
2Under the situation of diffractometer, the length of sample plummer can be chosen between 80mm to 100mm.Rotation monitor station of the present invention can accurately be installed in D8C easily
2But on the sample plummer of three translations of equipment, and the back is installed to D8C
2The function of equipment and accuracy of detection do not have any harmful effect.Among Fig. 1,1 is table top, promptly rotates the table top of monitor station, and 2 for the inclination rotating shaft, i.e. straight line AB, and 3 is detected sample, I
0And I is incident x ray and diffraction x ray.The O point is an x radiation exposure point (being the macro-stress check point).
Detected sample can be around the rotation of AB axle with the rotation monitor station, and to choose different side rake angle α, α can change between 0 ° to 90 °, and promptly detected sample surfaces and diffraction disk can be by mutual vertical change to being parallel to each other.This inner rotary monitor station can be rotated in table top 1, and rotation angle Φ can change between 0 ° to 360 °, so that detect the macro-stress on the different directions on the O point.The adjustment precision at α angle and Φ angle should be not less than 0.2.。
The welding newel is
The 10mmCu alloy, the internal diameter of outer shroud Ti alloy is 10mm.Weldment thickness is 5mm.Newel and outer shroud are closely cooperated, realize the differential expansion Diffusion Welding under the 850 degree conditions Celsius in a vacuum.
Be chosen in the variable gradient of measuring stress on the direction vertical in the 10mm scope with weld seam.According to the implementation step that the aforesaid inclination method of the present invention tiny area macro-stress detects, be the center with the weld seam, in ± 5mm scope, select 17 test points altogether, each test point all must be in α=0 °; α=16 °; α=24 °; Do one group of data under the inclination angle of α=30 °, and at the microscopically vernier focusing, experiment condition guarantees just the same.
Gained the results are shown among table 1 and Fig. 2, and 0 of horizontal ordinate is the soldered position among Fig. 2, and (+) direction is in the titanium alloy ring, and (-) direction is in the aldary post.As can be seen, all have tension in Cu alloy column and Ti alloy outer shroud from result of implementation, this is because the coefficient of thermal expansion of Cu alloy is bigger than Ti alloy, and the Cu alloy has produced the cause of bigger contraction during the cool to room temperature of welding back.In addition because Cu alloy ratio Ti alloy has bigger plasticity, so along with descend away from its stress value of weld seam more hurry up.
Table 1
| Distance/mm | -5.0 | -4.0 | -3.0 | -2.1 | -1.3 | -0.9 | -0.6 | -0.5 | -0.4 |
| Stress/Gpa | 0.015 | 0.016 | 0.02 | 0.04 | 0.07 | 0.12 | 0.16 | 0.21 | 0.25 |
| Distance/mm | 0.5 | 1.0 | 1.5 | 2.0 | 2.5 | 3.2 | 4.0 | 5.0 | |
| Stress/Gpa | 0.26 | 0.23 | 0.20 | 0.14 | 0.10 | 0.04 | 0.011 | 0.011 |
Diamond thin stress distribution unevenness with the growth of CVD method on the embodiment 3Mo substrate detects.
Adopt electronics to strengthen chemical vapor deposition (EA-CVD) method in 800～900 degrees centigrade of growing diamond polycrystalline film on the Mo substrate Celsius, its thickness is 0.3mm.
Detect implementation step by inclination method tiny area stress of the present invention, on film, choose 2mm * 2mm detection zone, 50 check points of picked at random in the district, each test point all must be in α=0 °; α=16 °; α=24 °; Do one group of data under the inclination angle of α=30 °, and at the microscopically vernier focusing, experiment condition guarantees, measures the macro-stress on the same direction just the same.
Calculate the occurrence probability of different stress values by testing result, in order to characterize the inconsistency (see figure 3) of detection zone internal stress size.
By among Fig. 3 as can be seen, the suffered compressive stress (negative value) that is in the diamond multicrystal film, this is because diamond film is littler than the thermal expansivity of Mo substrate, so the growth back will be subjected to the cause of the compression of substrate when cooling off.But can find out also that the value of compressive stress of each check point differs greatly in the inspection lateral areas (from-2GP extremely-11GP, mean value is 7.1GP), and different stress values are random stochastic distribution in detection zone, thereby reflect that the stress in the diamond thin not only derives from substrate, the influence of film self micromechanism unevenness also can not be ignored.
Claims (4)
1, a kind of x ray diffraction device that detects the tiny area macro-stress comprises an x x ray diffractometer x, is equipped with to be less than or equal to
0.1mm the online viewing microscope of primary ray collimator, sample and have can X, Y, the sample plummer and the laser ranging system of three translation motions of Z, it is characterized in that, the rotation monitor station is housed on the sample plummer; As the table top (1) of placing sample, table top (1) side and trimming bolt mesh said rotation monitor station by the disk that has the rotation angle scale, and can make table top (1) serves as that axle rotates and indicate rotation angle Φ with the Z direction; Diameter along table top (1) is provided with inclination rotating shaft (2), semicircle bevel protractor is housed on the Z direction, and the center of circle vertical with inclination rotating shaft (2), the plane of bevel protractor is in inclination rotating shaft (2), when table top (1) angle footage number when inclination rotating shaft (2) is rotated illustrates side rake angle α; Said side rake angle α is the angle of detected sample surfaces and diffraction disk.
According to the x ray diffraction device of the described detection tiny area of claim 1 macro-stress, it is characterized in that 2, the precision of rotation monitor station rotary manipulation is equal to or higher than 0.2 °.
3, a kind of method that detects the x x ray diffraction of tiny area macro-stress is characterized in that, uses the x x ray diffractometer x that is equipped with the rotation monitor station; The detection step has:
(1) the detected sample surfaces of adjusting on the rotation monitor station is vertical with x x ray diffractometer x diffraction circle platform, and the inclination rotating shaft is arranged on the intersection of diffraction disk and detected sample surfaces;
(2) select stress check point O at microscopically;
(3) by rotation angle Φ set the stress detection side to;
(4) determine side rake angle α, side rake angle α is detected sample surfaces and incident x ray I
0And the diffraction disk angulation of diffraction x ray I formation;
(5) observe stress check point O again at microscopically, adjust check point O and overlap with diffraction circle center;
(6) measure selected diffraction crystal face;
(7) selected stress check point O is repeated (5) and (6) step under different side rake angle α situations, obtain one group of 2 θ α data;
(8) calculate in the O point tiny area on the detected sample with roll axis AB vertical direction on the macro-stress value.
According to the method for the x x ray diffraction of the described detection tiny area of claim 3 macro-stress, it is characterized in that 4, side rake angle α selects α=0 °, α=16 °, α=24 °, α=30 ° to carry out duplicate measurements.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101986131A (en) * | 2010-09-21 | 2011-03-16 | 江苏赛福天钢绳有限公司 | Device for testing revolving performance of steel wire rope for elevator and testing method thereof |
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| CN101825212B (en) * | 2009-12-25 | 2013-02-13 | 中国计量科学研究院 | General-purpose spatial double-positioning rotating mechanism |
| CN102169033B (en) * | 2010-12-08 | 2013-04-03 | 北京科技大学 | Fixed-point non-destructive testing method for internal residual stress of aluminum alloy plate |
| CN102654468A (en) * | 2012-05-07 | 2012-09-05 | 上海交通大学 | Cloud picture measurement method representing shot blasting residual stress homogeneity |
| CN103900744B (en) * | 2014-03-18 | 2016-02-10 | 中国科学院上海微系统与信息技术研究所 | For the X-ray diffraction in-situ testing device through improving of battery charge and discharge process |
| CN110608827B (en) * | 2019-09-19 | 2020-12-25 | 西安交通大学 | Single crystal or directional crystal detection system based on monochromatic X-ray diffraction |
| CN110542506A (en) * | 2019-10-16 | 2019-12-06 | 丹东浩元仪器有限公司 | detection device and detection method for X-ray stress determinator |
| CN110542507B (en) * | 2019-10-16 | 2021-07-27 | 丹东浩元仪器有限公司 | Detection method of detection device of X-ray stress determinator |
| CN110779863B (en) * | 2019-11-06 | 2022-03-29 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Method for evaluating residual thermal stress of amorphous alloy thin strip |
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Cited By (2)
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| CN101986131A (en) * | 2010-09-21 | 2011-03-16 | 江苏赛福天钢绳有限公司 | Device for testing revolving performance of steel wire rope for elevator and testing method thereof |
| CN101986131B (en) * | 2010-09-21 | 2012-11-21 | 江苏赛福天钢索股份有限公司 | Device for testing revolving performance of steel wire rope for elevator and testing method thereof |
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