Summary of the invention
The object of the present invention is to provide a kind of layer-by-layer surface analysis device and methods of corrosion product based on X-ray diffractometer.
The present invention is the layer-by-layer surface analysis device and method of corrosion product based on X-ray diffractometer, is based on X-ray diffractometerThe layer-by-layer surface analysis device of corrosion product, have a sample stage 100, longitudinal dovetail guide 102 and first is arranged at 100 bottom of sample stageNut seat 101, sample stage 100 and reciprocating table 200 pass through longitudinal dovetail groove 201 on longitudinal dovetail guide 102 and reciprocating table 200Clearance fit connects, and is fixed with zigzag tread patterns motor 300,300 output shaft of zigzag tread patterns motor and first on reciprocating table 200Bevel gear 301 is fixedly connected, and first bevel gear 301 is engaged with second bevel gear 302, second bevel gear 302 and longitudinal ball wireThick stick 303 is fixedly connected, and longitudinal ball-screw 303 is connect with 101 clearance fit of the first nut seat of 100 bottom of sample stage, longitudinalDrive motor 300 is able to drive sample stage 100 and slides up and down along reciprocating table 200；Reciprocating table 200 passes through its bottom transverse direction swallowTail guide rail 202 is connect with 401 clearance fit of horizontal dovetail groove on pedestal 400, and laterally driven motor is fixed on pedestal 400500, which is fixedly connected with lateral ball-screw 501, and lateral ball-screw 501 passes through 400 bottom of pedestalBearing 402 is connect with 203 clearance fit of the second nut seat of 200 bottom of reciprocating table, and laterally driven motor 500 drives back and forthPlatform 200 horizontally slips along horizontal dovetail groove 401.
The method of the layer-by-layer surface analysis device of corrosion product based on X-ray diffractometer, the steps include:
(1) sample is installed:, will be to be measured on the basis of apparatus of the present invention are already fixed to conventional x-ray diffraction instrument specimen holderTo be measured face outwardly of block sample 700 is fixed in 100 front surface of sample stage；
(2) start X-ray diffractometer: according to conventional x-ray diffraction instrument Starting mode starting device, setting X-ray diffractionInstrument is initial and end of a period detection angles, scanning step, document storage location；
(3) detect position initialization: adjustment 100 position of sample stage makes a certain initial bit of X-ray emission window face sampleIt sets；
(4) it tests: closing X-ray diffractometer protective door, this object phase information is tested since default start angle；
(5) mobile test position: after upper pinpoint test, sample stage 100 drives sample 700 mobile, makes incident X-raysStop behind next position to be measured on 700 surface of face sample, guarantee the X-ray emission window face position to be measured, repeats the(4) step measures this object phase information；
(6) it continues to test: after second point is tested, repeating (5) step, sequentially determining sample surfaces are all to locationIt sets；
(7) rubbing down sample: after to all tested point measurements of specimen surface, sample 700 is removed, with objects such as abrasive paper for metallographIts surface for being tested of product rubbing down, to remove corrosion product；
(8) sample is installed again: after removal 700 surface layer of material of sample, according to the first one step process, again by sample 700It is secondary to be fixed on sample stage 100, it need to guarantee that 700 position and direction of sample being specifically fixed on sample stage 100 and first time are solidFixed is completely the same；
(9) it detects again: according to (3) step to (6) step, completing to examine at all positions to be measured of the second level of sampleIt surveys, it is desirable that each test point position should be overlapped with test point position is corresponded on the first level in the level；
(10) third, the section informations such as 4th are if desired detected, then repeatedly (8), (9) step；
(11) test terminates: after completing test, removing sample, resets simultaneously pass hull closure, clean out instrument and equipment；
(12) data processing: compound type and content on every bit are analyzed in each level, then in (X, Y, Z) three-coordinateIn system, each phase content at all test points is marked respectively.
Usefulness of the present invention are as follows: 1, can relatively accurately determine sample surfaces target location corrosion productType and content.2, it can intuitively reflect that corrosion product type and content change at sample surfaces different location and different depth.3, it overcomes and is limited to by X-ray penetration capacity and cause the corrosion product at sample surfaces deep place non-detectable tiredIt is difficult.
Detailed description of the invention
The layer-by-layer surface analysis device axonometric drawing of Fig. 1 corrosion product of the invention based on X-ray diffractometer, Fig. 2 present invention100 structure three-dimensional schematic diagram of sample stage, 100 structural front view of sample stage Fig. 3 of the invention, sample stage Fig. 4 of the invention100 the structure left view, 100 structure top view of sample stage Fig. 5 of the invention, 200 structure three-dimensional of reciprocating table Fig. 6 of the invention showIt is intended to, 200 structural front view of reciprocating table Fig. 7 of the invention, 200 the structure left view of reciprocating table Fig. 8 of the invention, this hair of Fig. 9Bright 200 structure top view of reciprocating table, the connection of zigzag tread patterns motor 300 Figure 10 of the invention and longitudinal ball-screw 303Structural schematic diagram, Figure 11 400 structure three-dimensional schematic diagram of pedestal of the invention, 400 structural front view of pedestal Figure 12 of the invention,400 the structure left view of pedestal Figure 13 of the invention, 400 structure top view of pedestal Figure 14 of the invention, cross Figure 15 of the inventionPass through 503 attachment structure schematic diagram of shaft coupling, the signal of Figure 16 detection process to drive motor 500 and lateral ball-screw 501Figure；Appended drawing reference and corresponding title are as follows: sample stage 100, the first nut seat 101, longitudinal dovetail guide 102, reciprocating table 200 are indulgedTo dovetail groove 201, lateral dovetail guide 202, the second nut seat 203, bearing 204, zigzag tread patterns motor 300, the first cone toothWheel 301, second bevel gear 302, longitudinal ball-screw 303, key 304, key 305, pedestal 400, horizontal dovetail groove 401, bearing402, countersunk screw hole 403, laterally driven motor 500, lateral ball-screw 501, shaft joint 502, X-ray diffractometer sampleFrame 600, sample 700 detect position 701, detect position 702.
Specific embodiment
The present invention is the layer-by-layer surface analysis device and method of corrosion product based on X-ray diffractometer, as shown in Figure 1, the dressSet including a sample stage 100, sample stage 100 and reciprocating table 200 by longitudinal dovetail guide 102 of 100 bottom of sample stage and201 clearance fit of longitudinal dovetail groove on reciprocating table 200 connects, and is fixed with zigzag tread patterns motor 300 on reciprocating table 200, shouldMotor 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 toothWheel 302 is fixedly connected with longitudinal ball-screw 303 again, and longitudinal ball-screw 303 passes through the bearing 204 of 200 bottom of reciprocating table, with101 clearance fit of the first nut seat of 100 bottom of sample stage connects, and zigzag tread patterns motor 300 may be implemented and drive sample stage100 purposes slided up and down along longitudinal dovetail groove 201；Reciprocating table 200 passes through its bottom transverse direction dovetail guide 202 and pedestal401 clearance fit of horizontal dovetail groove on 400 connects, and is fixed with laterally driven motor 500 on pedestal 400, the motor is defeatedShaft is fixedly connected with lateral ball-screw 501, and lateral ball-screw 501 passes through the bearing 402 of 400 bottom of pedestal, and reciprocal203 clearance fit of the second nut seat of 200 bottom of platform connects, and realizes that laterally driven motor 500 drives reciprocating table 200 along crossThe purpose to horizontally slip to dovetail groove 401 has countersunk screw hole 403 on pedestal 400, penetrates for pedestal 400 to be fixed on existing XOn line diffractometer specimen holder 600；Zigzag tread patterns motor 300 and laterally driven motor 500 pass through conducting wire and X-ray diffractionThe connection of instrument controller.
As shown in Fig. 2, the sample stage 100 be in cube structure, main view, left view and top view respectively as Fig. 3,Shown in Fig. 4 and Fig. 5；In main view shown in Fig. 3, there is one to be slightly higher than preceding table along 100 left side of sample stage and lower sideThere is first nut seat 101 at the boss in face, 100 rear surface center of sample stage, and 101 two sides of the first nut seat are two parallelLongitudinal dovetail guide 102.
As shown in fig. 6,200 3-D view of reciprocating table, main view, left view and top view are respectively such as Fig. 7, Fig. 8With shown in Fig. 9；The " U "-shaped plate in reciprocating table top has two longitudinal dovetail grooves 201 in two sides, is in the middle part of the reciprocating table" Fang " shape structure, and it is vertical with top " u "-shaped plane, it is a hollow cylinder axis among the upper side frame of " Fang " shape structureHold 204；There are two screw holes on the left of the upper surface of Contraband " character form structure lower frame, for fixing zigzag tread patterns motor 300；There is second nut seat 203 among the lower surface of " Fang " shape structure lower frame, 203 both sides of the second nut seat are two parallelLateral dovetail guide 202.
As shown in Figure 10,300 output shaft of zigzag tread patterns motor is connect with first bevel gear 301 by key 304, theOne bevel gear 301 engages with second bevel gear 302, and second bevel gear 302 is connect with longitudinal ball-screw 303 by key 305.
As shown in figure 11, the pedestal 400 is also in " Fang " shape structure, and 3-D view is as shown in figure 11, and its main viewFigure, left view and top view as shown in Figure 12, Figure 13 and Figure 14, there is a rectangular channel, rectangle respectively among 400 upper side frame of pedestalSlot two sides are two horizontal dovetail grooves 401；There is a hollow cylinder bearing 402 in 400 upper side frame lower surface of pedestal；Pedestal 400There are 8 countersunk screw holes 403 on lower frame, for pedestal 400 to be fixed on X-ray diffractometer specimen holder 600.
As shown in figure 15, the laterally driven motor 500 is connect with lateral ball-screw 501 by shaft joint 502.
Further, what the plane that described two longitudinal dovetail grooves 201 determine should be determined with two horizontal dovetail grooves 401Plane is vertical.
Further, the X-ray diffractometer controller needs in current conventional x-ray diffraction instrument control system-basedIncrease can individually control zigzag tread patterns motor 300 and laterally driven motor 500 opens, stop and forward and backward function.
It is fixed assuming that the invention equipment has passed through countersunk screw hole 403 with conventional x-ray diffraction instrument specimen holder, and X is penetratedLine diffractometer controller can correctly control zigzag tread patterns motor 300 and laterally driven motor 500 opens, stop and forward and backward.The method of the layer-by-layer surface analysis device of corrosion product then based on X-ray diffractometer is as follows:
Step 1: installation sample: size is less than to the surface to be measured of the bulk sample 700 of 100 upper surface size of sample stageOutward, side is bonded 100 left side of sample stage and downside boss respectively, before being fixed on sample stage 100 using materials such as double-sided adhesivesOn surface, it need to guarantee that sample surface to be measured is parallel to each other in the plane that two longitudinal dovetail grooves 201 determine.
Step 2: starting X-ray diffractometer: power supply is opened, according to conventional x-ray diffraction instrument Starting mode starting device,And setting X-ray diffractometer is initial and end of a period detection angles, scanning step, document storage location etc. according to a conventional method.
Step 3: detection position initialization: controlling zigzag tread patterns motor 300 and cross by X-ray diffractometer controllerTo drive motor 500,100 position of sample stage is adjusted, a certain initial position of X-ray emission window face sample, such as Figure 16 are madeShown detection position 701.
Step 4: test: closing X-ray diffractometer protective door, this object phase information is tested since default start angle.
Step 5: mobile test position: after upper pinpoint test, X-ray diffractometer controller controls zigzag tread patterns electricityMotivation 300 and laterally driven motor 500 work, and sample stage 100 drives sample 700 mobile, make incident X-rays face sampleStop behind next position to be measured on 700 surfaces, detect position 702 as shown in figure 15, repeats four-step method, measure the objectPhase information.
Step 6: continuing to test: after second point is tested, repeating the 5th step process, such as signified according to Figure 15 arrowMeasure route, all positions to be measured of sequentially determining sample surfaces.
Step 7: rubbing down sample: after to all tested point measurements of specimen surface, that is, obtaining the sample the first level objectPhase 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 withCertain thickness corrosion product is removed, rubbing down depth must guarantee removal depending on the precision of extent of corrosion and detection depthDepth of material is uniform.
Step 8: installing sample again: after removal 700 surface layer of material of sample, its surface scum being cleaned out, is pressedAccording to the first one step process, sample 700 is fixed on again on sample stage 100, in addition to meeting the requirement in the first step, also needs to guarantee thisSecondary 700 position and direction of sample being fixed on sample stage 100 are fixed consistent with first time.
Step 9: detecting again: according to third step to the 6th one step process, completing at all positions to be measured of the second level of sampleDetection, it is desirable that each test point position should be overlapped with test point position is corresponded on the first level in the level.
Step 10: if desired detect third, the section informations such as 4th, then repeatedly the eight, the 9th step.
Step 11: test terminates: after completing test, removing sample, reset simultaneously pass hull closure, clean out instrument and setIt is standby.
Step 12: data processing: using X ray diffracting data interpretation software, analyze respectively every in each levelA little upper compound type and content；Again in (X, Y, Z) system of 3 axes, each object at all test points is marked respectively and is mutually containedAmount can intuitively, accurately determine at sample surfaces different location and different depth how much is a certain content of material.
The layer-by-layer surface analysis device and method of the corrosion product provided by the invention based on X-ray diffractometer has been done in detail aboveIt describes in detail bright.For those skilled in the art, according to the thought of the present invention, having in specific embodiments and applications canIt can change.So limitation of the present invention should not be interpreted as this specification.Appointing under basic thought of the present invention limitationWhat, which changes, belongs within scope, and scope of patent protection proper right of the invention requires limitation.