CN106645238A - Layer-by-layer analyzing device for corrosion products based on X-ray diffractometer and method - Google Patents
Layer-by-layer analyzing device for corrosion products based on X-ray diffractometer and method Download PDFInfo
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- CN106645238A CN106645238A CN201710135458.1A CN201710135458A CN106645238A CN 106645238 A CN106645238 A CN 106645238A CN 201710135458 A CN201710135458 A CN 201710135458A CN 106645238 A CN106645238 A CN 106645238A
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- G—PHYSICS
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- 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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Abstract
The invention discloses a layer-by-layer analyzing device for corrosion products based on an X-ray diffractometer and a method. The device comprises a rectangular sample stage and electric motors, wherein one electric motor drives one corresponding lead screw and drives the sample stage to vertically slide along a longitudinal reciprocating table; the longitudinal reciprocating table is connected with the other lead screw, and is driven by the other electric motor to laterally slide along a transverse reciprocating table; the transverse reciprocating table is fixed on a sample rack of an existing X-ray diffractometer; the starting and the stopping of the two electric motors are controlled by an X-ray diffractometer controller. The operation method comprises the following steps: adjusting the position of a sample by the lead screws; detecting all the positions on the surface of the sample fixed on the sample stage one by one according to a conventional method for measuring phases by the X-ray diffractometer; then removing a layer of material on the surface of the sample, detecting the position detected in the first time again according to the method, and repeating the process for multiple times; finally, analyzing the kinds and the contents of the phases at all test points, and drawing to obtain the kind and content information of corrosion products on corrosion levels with different depths relatively accurately and visually.
Description
Technical field
The present invention relates to the technology using X-ray diffraction to material corrosion product analysis.
Background technology
After sample corrosion, the species and each phase content for detecting surface corrosion product is analysis corrosion mechanism, control corrosion rate
The important step of process.For the material phase analysis of block sample surfaces corrosion product, current conventional means is by X-ray diffraction
Instrument, based on coherent diffraction principle and Bragg equation condition are strengthened, and specimen surface is detected, then are asked for by corresponding analysis software
The thing phase information of measurand.
But there is problems with existing method:(1)Sampling location is random, information fuzzy:X-ray beam spot is irradiated to sample table
Face position is difficult to be accurately positioned, it is more difficult to be inferred to the thing phase information of target area.(2)Sampling area is little, and specimen surface information is not
Comprehensively:Project the X-ray beam spot about 1mm of specimen surface2, the information of acquisition can not comprehensively reflect specimen surface corrosion product
Information;(3)X-ray penetration depth is limited, and information is not comprehensive on corrosion layer depth direction:Sample etches layer depth often reaches hundreds of
Micron, it is even thicker, and different corrosion layer thing is mutually often different, thing mutually detection X-ray despite hard X ray, but it is penetrated
Sample depth is still limited, is typically only capable of reflecting thing phase information in the range of tens micrometer depths, causes different depth corrosion layer to be believed
Breath is difficult to embody.
The content of the invention
It is an object of the invention to provide a kind of corrosion product based on X-ray diffractometer successively surface analysis device and method.
The present invention is based on the corrosion product successively surface analysis device and method of X-ray diffractometer, based on X-ray diffractometer
Corrosion product successively surface analysis device, have a sample stage 100, longitudinal dovetail guide 102 and first is arranged at the bottom of sample stage 100
Nut seat 101, sample stage 100 is with reciprocating table 200 by the longitudinal dovetail groove 201 on longitudinal dovetail guide 102 and reciprocating table 200
Gap is connected, and zigzag tread patterns motor 300, the output shaft of zigzag tread patterns motor 300 and first are fixed with reciprocating table 200
Bevel gear 301 is fixedly connected, and first bevel gear 301 is engaged with second bevel gear 302, second bevel gear 302 and longitudinal ball wire
Thick stick 303 is fixedly connected, and longitudinal ball-screw 303 is connected with the gap of the first nut seat 101 of the bottom of sample stage 100, longitudinal direction
Drive motor 300 can drive sample stage 100 to slide up and down along reciprocating table 200;Reciprocating table 200 passes through the horizontal swallow in its bottom
Tail guide rail 202 is connected with the gap of horizontal dovetail groove 401 on base 400, and laterally driven motor is fixed with base 400
500, the motor output shaft is fixedly connected with horizontal ball-screw 501, and horizontal ball-screw 501 is through the bottom of base 400
Bearing 402, is connected with the gap of the second nut seat 203 of the bottom of reciprocating table 200, and laterally driven motor 500 drives back and forth
Platform 200 horizontally slips along horizontal dovetail groove 401.
The method of the successively surface analysis device of the corrosion product based on X-ray diffractometer, its step is:
(1)Sample is installed:On the basis of apparatus of the present invention are already fixed to conventional x-ray diffraction instrument specimen holder, by block to be measured
To be measured the facing outwardly of sample 700 is fixed on the front surface of sample stage 100;
(2)Start X-ray diffractometer:According at the beginning of conventional x-ray diffraction instrument Starting mode starting device, setting X-ray diffractometer
Begin and end of a period detection angles, scanning step, document storage location;
(3)Test position is initialized:Adjustment sample stage 100 position, makes X-ray emission window just to a certain initial position of sample;
(4)Test:X-ray diffractometer protective door is closed, starts to test the thing phase information from default start angle;
(5)Mobile test position:After upper pinpoint test terminates, sample stage 100 drives sample 700 to move, and makes incident X-rays just right
Stop behind the position next to be measured on the surface of sample 700, it is ensured that X-ray emission window repeats the just to the position to be measured(4)Step
Suddenly, the thing phase information is determined;
(6)Continue to detect:After second point test terminates, repeat the(5)Step, all positions to be measured of sequentially determining sample surfaces;
(7)Rubbing down sample:After all tested point measurements of specimen surface terminate, sample 700 is removed, thrown with abrasive paper for metallograph and other items
The surface of its tested mistake is ground, to remove corrosion product;
(8)Sample is installed again:It is according to the first one step process, sample 700 is solid again after removing the surface layer of material of sample 700
On sample stage 100, need to ensure what the position of sample 700 being specifically fixed on sample stage 100 and direction and first time were fixed
It is completely the same;
(9)Detect again:According to(3)Step is to(6)Step, completes to be detected at all positions to be measured of the aspect of sample second,
It is required that each test point position should test point position coincidence corresponding with the first level in the aspect;
(10)If desired detection the 3rd, fourth class section information, then repeatedly the(8),(9)Step;
(11)Test terminates:After completing test, sample is removed, resetted and pass hull closure, clean out instrument and equipment;
(12)Data processing:Compound type and content on every bit are analyzed in each aspect, then in (X, Y, Z) system of 3 axes
In, each phase content at all test points is marked respectively.
Usefulness of the present invention is:1st, sample surfaces target location corrosion product can relatively accurately be determined
Species and content.2nd, corrosion product species and content change at sample surfaces diverse location and different depth can intuitively be reflected.
3rd, overcome and limited to and cause the corrosion product at sample surfaces deep place non-detectable tired by X-ray penetration capacity
It is difficult.
Description of the drawings
Corrosion product based on the X-ray diffractometer successively surface analysis device axonometric drawing of Fig. 1 present invention, Fig. 2 is of the invention
The structure three-dimensional schematic diagram of sample stage 100, Fig. 3 the present invention the structural front view of sample stage 100, Fig. 4 the present invention sample stage
100 structure left views, the structure top view of sample stage 100 of Fig. 5 present invention, the structure three-dimensional of reciprocating table 200 of Fig. 6 present invention shows
Be intended to, Fig. 7 the present invention the structural front view of reciprocating table 200, Fig. 8 the present invention the structure left view of reciprocating table 200, Fig. 9 this
The bright structure top view of reciprocating table 200, the zigzag tread patterns motor 300 of Figure 10 present invention and the connection of longitudinal direction ball-screw 303
Structural representation, the structure three-dimensional schematic diagram of base 400 of Figure 11 present invention, the structural front view of base 400 of Figure 12 present invention,
The structure left view of base 400 of Figure 13 present invention, the structure top view of base 400 of Figure 14 present invention, the horizontal stroke of Figure 15 present invention
To drive motor 500 with horizontal ball-screw 501 by the attachment structure schematic diagram of shaft coupling 503, Figure 16 detection process is illustrated
Figure;Reference and correspondence are entitled:Sample stage 100, the first nut seat 101, longitudinal dovetail guide 102, reciprocating table 200 is indulged
To dovetail groove 201, horizontal dovetail guide 202, the second nut seat 203, bearing 204, zigzag tread patterns motor 300, the first cone tooth
Wheel 301, second bevel gear 302, longitudinal ball-screw 303, key 304, key 305, base 400, horizontal dovetail groove 401, bearing
402, countersunk screw hole 403, laterally driven motor 500, horizontal ball-screw 501, shaft joint 502, X-ray diffractometer sample
Frame 600, sample 700, test position 701, test position 702.
Specific embodiment
The present invention is based on the corrosion product successively surface analysis device and method of X-ray diffractometer, as shown in figure 1, the dress
Put including a sample stage 100, sample stage 100 and reciprocating table 200 by longitudinal dovetail guide 102 of the bottom of sample stage 100 and
The gap of longitudinal dovetail groove 201 on reciprocating table 200 is connected, and zigzag tread patterns motor 300 is fixed with reciprocating table 200, should
Motor output shaft is fixedly connected with first bevel gear 301, and first bevel gear 301 is engaged with second bevel gear 302, the second cone tooth
Wheel 302 is fixedly connected again with longitudinal ball-screw 303, and longitudinal ball-screw 303 passes through the bearing 204 of the bottom of reciprocating table 200, with
The gap of first nut seat 101 of the bottom of sample stage 100 is connected, it is possible to achieve zigzag tread patterns motor 300 drives sample stage
100 purposes slided up and down along longitudinal dovetail groove 201;Reciprocating table 200 is by the horizontal dovetail guide 202 in its bottom and base
The gap of horizontal dovetail groove 401 on 400 is connected, and laterally driven motor 500 is fixed with base 400, and the motor is defeated
Shaft is fixedly connected with horizontal ball-screw 501, horizontal ball-screw 501 through the bottom of base 400 bearing 402, it is and reciprocal
The gap of second nut seat 203 of the bottom of platform 200 is connected, and realizes that laterally driven motor 500 drives reciprocating table 200 along horizontal stroke
To the purpose that dovetail groove 401 horizontally slips, there is countersunk screw hole 403 on base 400, penetrate for base 400 to be fixed on into existing X
On line diffractometer specimen holder 600;Zigzag tread patterns motor 300 and laterally driven motor 500 are by wire and X-ray diffraction
Instrument controller connects.
As shown in Fig. 2 the sample stage 100 be in cube structure, its front view, left view and top view respectively as Fig. 3,
Shown in Fig. 4 and Fig. 5;In front view shown in Fig. 3, table before having to be slightly higher than along the left side of sample stage 100 and lower side
The boss in face, centre of surface has first nut seat 101 after sample stage 100, and the both sides of the first nut seat 101 are two parallel
Longitudinal dovetail guide 102.
As shown in fig. 6, the 3-D view of the reciprocating table 200, its front view, left view and top view are respectively such as Fig. 7, Fig. 8
With shown in Fig. 9;The " U "-shaped tabular in reciprocating table top, has two longitudinal dovetail grooves 201 in both sides, and the reciprocating table middle part is in
" Contraband " character form structure, and it is vertical with top " u "-shaped plane, it is a hollow cylinder axle in the middle of the upper side frame of " Contraband " character form structure
Hold 204;There are two screw holes in the upper surface left side of Contraband " character form structure lower frame, for fixing zigzag tread patterns motor 300;
There is second nut seat 203 in the middle of the lower surface of " Contraband " character form structure lower frame, the both sides of the second nut seat 203 are two parallel
Horizontal dovetail guide 202.
As shown in Figure 10, the output shaft of zigzag tread patterns motor 300 is connected with first bevel gear 301 by key 304, the
One bevel gear 301 engages with second bevel gear 302, and second bevel gear 302 is connected with longitudinal ball-screw 303 by key 305.
As shown in figure 11, the base 400 is also in " Contraband " character form structure, and its 3-D view is as shown in figure 11, and its main view
Figure, left view and top view as shown in Figure 12, Figure 13 and Figure 14, there is a rectangular channel, rectangle respectively in the middle of the upper side frame of base 400
Groove both sides are two horizontal dovetail grooves 401;The upper side frame lower surface of base 400 has a hollow cylinder bearing 402;Base 400
There are 8 countersunk screw holes 403 on lower frame, for base 400 to be fixed on into X-ray diffractometer specimen holder 600.
As shown in figure 15, the laterally driven motor 500 is connected with horizontal ball-screw 501 by shaft joint 502.
Further, described two longitudinal dovetail grooves 201 determine plane should determine with two horizontal dovetail grooves 401
Plane is vertical.
Further, the X-ray diffractometer controller is needed in current conventional x-ray diffraction instrument control system-based
Increase can individually control zigzag tread patterns motor 300 and laterally driven motor 500 is opened, stopped and forward and backward function.
Assume that the invention equipment is fixed by countersunk screw hole 403 with conventional x-ray diffraction instrument specimen holder, and X is penetrated
Line diffractometer controller can correctly control zigzag tread patterns motor 300 and laterally driven motor 500 is opened, stopped and forward and backward.
Method then based on the corrosion product successively surface analysis device of X-ray diffractometer is as follows:
The first step:Sample is installed:By the surface to be measured for being smaller in size than the bulk sample 700 of the upper surface size of sample stage 100 outwards,
Its side is fitted respectively the left side of sample stage 100 and downside boss, and using materials such as double faced adhesive tapes the front surface of sample stage 100 is fixed on
On, need to ensure that sample surface to be measured is parallel to each other in the plane that two longitudinal dovetail grooves 201 determine.
Second step:Start X-ray diffractometer:Turn on the power, according to conventional x-ray diffraction instrument Starting mode starting device,
And set that X-ray diffractometer is initial according to a conventional method and end of a period detection angles, scanning step, document storage location etc..
3rd step:Test position is initialized:Zigzag tread patterns motor 300 and horizontal stroke are controlled by X-ray diffractometer controller
To drive motor 500, adjustment sample stage 100 position, make X-ray emission window just to a certain initial position of sample, such as Figure 16
Shown test position 701.
4th step:Test:X-ray diffractometer protective door is closed, starts to test the thing phase information from default start angle.
5th step:Mobile test position:After upper pinpoint test terminates, X-ray diffractometer controller control zigzag tread patterns electricity
Motivation 300 and laterally driven motor 500 work, and sample stage 100 drives sample 700 to move, and makes incident X-rays just to sample
Stop behind the position next to be measured on 700 surfaces, test position as shown in figure 15 702, repeat four-step method, determine the thing
Phase information.
6th step:Continue to detect:After second point test terminates, repeat the 5th step process, such as according to Figure 15 arrow indications
Measurement route, all positions to be measured of sequentially determining sample surfaces.
7th step:Rubbing down sample:After all tested point measurements of specimen surface terminate, that is, obtain the sample the first level thing
Phase information, then open X-ray diffractometer protective door, remove sample 700, with its measured surface of abrasive paper for metallograph and other items rubbing down with
Certain thickness corrosion product is removed, depending on precision of the rubbing down depth according to extent of corrosion and detection depth, but must ensure to remove
Depth of material is uniform.
8th step:Sample is installed again:After removing the surface layer of material of sample 700, its surface scum is cleaned out, pressed
According to the first one step process, sample 700 is fixed on again on sample stage 100, in addition to the requirement in the first step is met, also needs to ensure this
The secondary position of sample 700 being fixed on sample stage 100 and direction are consistent with what first time was fixed.
9th step:Detect again:According to the 3rd step to the 6th one step process, complete at all positions to be measured of the aspect of sample second
Detection, it is desirable to which each test point position should test point position coincidence corresponding with the first level in the aspect.
Tenth step:If desired detection the 3rd, fourth class section information, then repeatedly the eight, the 9th step.
11st step:Test terminates:After completing test, sample is removed, resetted and pass hull closure, cleaned out instrument and set
It is standby.
12nd step:Data processing:Using X ray diffracting data interpretation software, analyze every in each aspect respectively
Any upper compound type and content;Again in (X, Y, Z) system of 3 axes, each thing at all test points is marked respectively and is mutually contained
Amount, you can intuitively, accurately determine that a certain content of material is how many at sample surfaces diverse location and different depth.
Successively surface analysis device and method has done in detail the corrosion product based on X-ray diffractometer for providing the present invention above
Describe in detail bright.For those skilled in the art, according to the thought of the present invention, having in specific embodiments and applications can
Can change.So, this specification should not be interpreted as limitation of the present invention.Appointing in the case where basic thought of the present invention is limited
What changes belongs within scope, and the scope of patent protection proper right of the present invention requires to limit.
Claims (4)
1. the corrosion product successively surface analysis device based on X-ray diffractometer, there is a sample stage(100), it is characterised in that:Sample
Sample platform(100)Longitudinal dovetail guide is arranged at bottom(102)With the first nut seat(101), sample stage(100)With reciprocating table(200)It is logical
Cross longitudinal dovetail guide(102)And reciprocating table(200)On longitudinal dovetail groove(201)Gap is connected, reciprocating table(200)On
It is fixed with zigzag tread patterns motor(300), zigzag tread patterns motor(300)Output shaft and first bevel gear(301)It is fixedly connected,
First bevel gear(301)With second bevel gear(302)Engagement, second bevel gear(302)With longitudinal ball-screw(303)It is fixed to connect
Connect, longitudinal ball-screw(303)With sample stage(100)First nut seat of bottom(101)Gap is connected, zigzag tread patterns electricity
Motivation(300)Sample stage can be driven(100)Along reciprocating table(200)Slide up and down;Reciprocating table(200)It is horizontal by its bottom
Dovetail guide(202)With base(400)On horizontal dovetail groove(401)Gap is connected, base(400)On be fixed with laterally
Drive motor(500), the motor output shaft and horizontal ball-screw(501)It is fixedly connected, horizontal ball-screw(501)Wear
Cross base(400)The bearing of bottom(402), with reciprocating table(200)Second nut seat of bottom(203)Gap is connected, horizontal
To drive motor(500)Drive reciprocating table(200)Along horizontal dovetail groove(401)Horizontally slip.
2. the corrosion product based on X-ray diffractometer according to claim 1 successively surface analysis device, it is characterised in that edge
Sample stage(100)Left side and lower side have a boss for being slightly higher than front surface, sample stage(100)Afterwards centre of surface has
One the first nut seat(101), the first nut seat(101)Both sides are two parallel longitudinal dovetail guides(102).
3. the corrosion product based on X-ray diffractometer according to claim 1 successively surface analysis device, it is characterised in that institute
State two longitudinal dovetail grooves(201)It is determined that plane should be with two horizontal dovetail grooves(401)It is determined that plane it is vertical.
4. based on X-ray diffractometer corrosion product successively surface analysis device method, its step is:
(1)Sample is installed:On the basis of apparatus of the present invention are already fixed to conventional x-ray diffraction instrument specimen holder, by block to be measured
Sample(700)To be measured facing outwardly be fixed on sample stage(100)On front surface;
(2)Start X-ray diffractometer:According at the beginning of conventional x-ray diffraction instrument Starting mode starting device, setting X-ray diffractometer
Begin and end of a period detection angles, scanning step, document storage location;
(3)Test position is initialized:Adjustment sample stage(100)Position, makes X-ray emission window just to a certain initial bit of sample
Put;
(4)Test:X-ray diffractometer protective door is closed, starts to test the thing phase information from default start angle;
(5)Mobile test position:After upper pinpoint test terminates, sample stage(100)Drive sample(700)It is mobile, make incident X-rays
Just to sample(700)Stop behind the position next to be measured on surface, it is ensured that X-ray emission window repeats just to the position to be measured
The(4)Step, determines the thing phase information;
(6)Continue to detect:After second point test terminates, repeat the(5)Step, all positions to be measured of sequentially determining sample surfaces;
(7)Rubbing down sample:After all tested point measurements of specimen surface terminate, sample is removed(700), with abrasive paper for metallograph and other items
The surface of rubbing down its tested mistake, to remove corrosion product;
(8)Sample is installed again:Remove sample(700)After the layer of material of surface, according to the first one step process, by sample(700)Again
It is secondary to be fixed on sample stage(100)On, need to ensure specifically to be fixed on sample stage(100)On sample(700)Position and direction and the
That what is once fixed is completely the same;
(9)Detect again:According to(3)Step is to(6)Step, completes to be detected at all positions to be measured of the aspect of sample second,
It is required that each test point position should test point position coincidence corresponding with the first level in the aspect;
(10)If desired detection the 3rd, fourth class section information, then repeatedly the(8),(9)Step;
(11)Test terminates:After completing test, sample is removed, resetted and pass hull closure, clean out instrument and equipment;
(12)Data processing:Compound type and content on every bit are analyzed in each aspect, then in (X, Y, Z) system of 3 axes
In, each phase content at all test points is marked respectively.
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CN201710135458.1A CN106645238B (en) | 2017-03-09 | 2017-03-09 | The layer-by-layer surface analysis device and method of corrosion product based on X-ray diffractometer |
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CN201710135458.1A CN106645238B (en) | 2017-03-09 | 2017-03-09 | The layer-by-layer surface analysis device and method of corrosion product based on X-ray diffractometer |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112710681A (en) * | 2020-12-21 | 2021-04-27 | 中南大学 | Experimental device for solidification behavior is observed to normal position |
EP3940376A4 (en) * | 2019-05-15 | 2022-06-15 | Lg Chem, Ltd. | Stage device for xrd measurement of battery |
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CN202330313U (en) * | 2011-11-23 | 2012-07-11 | 中国科学院上海应用物理研究所 | Cooling sample platform of film X-ray diffractometer and X-ray diffractometer |
CN103901062A (en) * | 2014-03-05 | 2014-07-02 | 中国科学院青海盐湖研究所 | Sample platform mounted on powder X-ray diffractometer and used for testing solid block-shaped sample |
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CN2840028Y (en) * | 2005-10-17 | 2006-11-22 | 马鞍山钢铁股份有限公司 | Rotary sample table for X-ray diffractometer |
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CN202330313U (en) * | 2011-11-23 | 2012-07-11 | 中国科学院上海应用物理研究所 | Cooling sample platform of film X-ray diffractometer and X-ray diffractometer |
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