CN207528521U - The device for preparing X ray nanometer CT metal micro-test samples based on local electrochemical etching - Google Patents
The device for preparing X ray nanometer CT metal micro-test samples based on local electrochemical etching Download PDFInfo
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- CN207528521U CN207528521U CN201721150007.7U CN201721150007U CN207528521U CN 207528521 U CN207528521 U CN 207528521U CN 201721150007 U CN201721150007 U CN 201721150007U CN 207528521 U CN207528521 U CN 207528521U
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Abstract
The utility model discloses a kind of devices of the preparation nanometer CT metal micro-test samples based on local electrochemical etching, and including precise position control unit, electrochemical etching unit, real time monitoring unit, the precise position control unit is used for the translation of sample；The electrochemical etching unit is used for accurate etching sample, obtains required structure；The state is acquired imaging by the real time monitoring unit for observing the etching state of sample in real time.The utility model convenient and efficient, inexpensive can prepare that diameter is only tens of or a few micrometers of metal microtrabeculae samples and complicated shape such as dog bone shape in-situ mechanical test micro-test sample by electrochemistry localized etching, suitable for the preparation of the X ray nanometer CT samples of most metal or alloy, it solves the sample preparation problem of metal material nanometer CT three-dimensional microstructures analysis, has great importance to the popularization and application for promoting X ray Micro-CT scanning.
Description
Technical field：
The utility model belongs to metal micro-test sample manufacture field, and in particular to a kind of preparation based on local electrochemical etching
The device of X ray nanometer CT metal micro-test samples.
Background technology
X ray computer tomoscan (Computed Tomography, CT) technology can be to detecting object three-dimensional perspective
Noninvasive imaging has important application in fields such as medical diagnosis, scientific research and industrial detections.In recent years, with X ray
The high speed development in source, detector and computer technology, the spatial resolution of X ray CT are continuously improved, have reached micron and even received
Rice magnitude.At present, the nanometer CT (highest resolution reaches 50nm) of commercialized Laboratory X-ray light source is gradually mounted to
In the laboratories such as investigation of materials, oil exploration, energy development.
The visual field of X ray CT reduces with the raising of spatial resolution.If the projected image resolution ratio of nanometer CT is
1024 × 1024 pixels, then when spatial resolution is 150nm, visual field width is 65 μm；And when resolution ratio reaches 50nm,
Visual field width is only 15 μm.During CT scan, sample must around visual field central axis and rotation overall process cannot exceed regard
.This requires the external body diameter in the range of sample field height is necessarily less than 65 μm (big visual field patterns) or 15 μm of (height
Resolution pattern).On the other hand, metal material is stronger to X-ray absorption, and sample size is also further by X-ray transparent rate
Constraint.For example, for 8.0keV (Cu KαRadiation) Laboratory X-ray light source, the maximum sample thickness of Cu, Ni is 40 μm, Ti
It it is 20 μm, Fe, Co etc. are only 8 μm.2 points of constraints more than considering, how to prepare metal micro-test sample is X ray nanometer CT
The key of three-dimensional structure characterization.
Preparing micro-meter scale sample is mainly the following method at present：(1) focused ion beam (Focused Ion
Beam, FIB) it is that the fine micro Process of nanoscale is carried out, but its processing efficiency is relatively low to material using high intensity converging ion beam.
It is prepared using FIB more than 10 μm3Micron sample be very time-consuming.FIB system is expensive simultaneously, operation expense
Height is not suitable for the processing of a large amount of micron samples.(2) pulse laser ablation compared with FIB, can quickly remove lot of materials, but
The fuel factor of process may damage sample extexine, form tens microns of wide heat affected areas, and machining accuracy is relatively
It is low.(3) microdissection technology is softer to quality commonly used in cutting the hard materials such as the square column type ceramics of micro-meter scale, silicon chip
Metal material be also easy to produce apparent mechanical damage.Therefore, these methods be not suitable for preparing metal material nanometer CT it is micro-
Sample.
A potential forward position application of X ray nanometer CT is to carry out the test of metal material in-situ mechanical and fracture damage mechanism
Research.This requirement prepares the micro-stretching sample of dog bone shape, and in-between gauge length section diameter meets nanometer CT test requests, and
Head is larger to be used to matched with collet by load transmission to gauge length section.Existing micro-processing technology fail it is convenient and efficient, low into
Locally prepare the micro- test sample in such original position.
Utility model content
The purpose of this utility model is to provide it is a kind of based on local electrochemical etching to prepare X ray nanometer CT metals micro-
The device of sample.The utility model can easily prepare the X ray nanometer CT microtrabeculae samples of most metal or alloy；It can be accurate
It determines area-of-interest, and makes area-of-interest localized etching；The micro- examination of metal of complicated shape such as dog bone shape can be prepared
Sample, for in-situ mechanical test and crack initiation, extensive diagnostic.
The above-mentioned purpose of the utility model is achieved through the following technical solutions：
The device for preparing X ray nanometer CT metal micro-test samples based on local electrochemical etching, including precise position control
Unit, electrochemical etching unit, real time monitoring unit, the precise position control unit are used for the translation of sample；The electricity
Chemical etching unit is used for accurate etching sample, obtains required structure；The real time monitoring unit is for observation sample in real time
Etching state, and the state is acquired imaging.
Preferably, precise position control unit includes uniaxial motorized precision translation stage, the stepping motor for carrying spherical guide, Gu
Upper clamp plate, lower clamp plate and the control module of control motorized precision translation stage rate travel and its distance of random sample product clamping piece, stepping
Motor drives motorized precision translation stage movement, and upper clamp plate, lower clamp plate are fixed on motorized precision translation stage, and precise position control unit is accurate
Sample position is controlled, electrolyte membrane uniform fold is made to realize that fixed point etching or automatic cycle are back and forth transported in interested region
It is dynamic to make etching more uniform.
Preferably, the power supply of electrochemical etching unit uses Digital DC Voltage-stabilized Power Source, and power cathode connects copper conductive electrode,
The fixed specimen holder gripping member of positive pole connection；Copper conductive electrode connects platinum filament coil first end, platinum filament coil second end setting cyclization
Shape structure, and electrolyte is coated, copper conduction extremely block is placed on pedestal.
Preferably, real time monitoring unit includes the ccd image harvester, fixing bracket, the LED rings that set zoomable camera lens
Shape light source adjusts accurate burnt spiral, wherein, ccd image harvester is fixed on fixing bracket, by being arranged on fixing bracket
The accurate burnt spiral of adjusting drive ccd image harvester longitudinal translation, needed for LED annular light sources supplement ccd image harvester
Light, ccd image harvester are acquired and are imaged in real time to the etching state of sample.
The basic principle of the utility model is that metal buttress shaft (connecing anode) by being inserted into platinum filament coil center and coil (connect
Cathode) between electrolyte membrane in electrochemical reaction, metal in electrolyte membrane overlay area is made constantly to dissolve, realize metal it is thin
The localized etching of column, the metal micro-test sample for being only tens of or even several microns until obtaining diameter.
Compared with prior art, the utility model has following remarkable advantage：(1) platinum filament coil chemical property is stablized, and prolongs
Malleability is good, as cathode, is not involved in chemically reacting, is not easy to be corroded by strong acid and strong base, can use for a long time；(2) sample position
Control software can realize that micron accuracy positions, and realize the localized etching of area-of-interest；(3) sample position control software can control
Sample automatic cycle moves back and forth, and makes electrochemical etching local more uniform；(4) can observe in real time sample etching state and into
Journey controls sample surfaces quality；(5) can prepare diameter be only tens of a few micrometers of metal microtrabeculae samples or dog bone shape it is micro-
Type in-situ mechanical test sample, and can realize the etching specific interested position of sample.
Description of the drawings
Fig. 1 is the structure diagram of device described in the utility model.
Fig. 2 is the fine copper micro-test sample pictorial diagram prepared using described device.
Fig. 3 is the pure nickel micro-test sample pictorial diagram prepared using described device.
Specific embodiment
The concrete structure and embodiment of the utility model are further described with reference to the accompanying drawings and examples.
The structure of the utility model is as shown in Figure 1, whole device includes precise position control unit, electrochemical etching list
Member, real time monitoring unit.The precise position control unit includes motorized precision translation stage 1, stepping motor 2, stepping motor and drives
Dynamic device 3, for fixing the upper clamp plate 4 of sample, lower clamp plate 5 and control module 6.Electronic mobile platform 1 is provided with precise cross-shaped
Spherical guide 8, positioning accuracy are 0.5 μm.The control module 6 can realize the micron order movement of electric platforms, be accurately positioned office
The position of domain etching.Meanwhile for the uniformity for improving local etching, the control module 6 can make sample in a certain range
Automatic cycle moves back and forth.
Described real time monitoring unit include setting the ccd image harvester 10 of zoomable camera lens 9, fixing bracket 12,
LED annular light sources 13 adjust accurate burnt spiral 14, wherein, ccd image harvester 10 is fixed on fixing bracket 12, by setting
It puts the accurate burnt spiral 14 of the adjusting on fixing bracket 12 and drives 10 longitudinal translation of ccd image harvester, LED annular light sources 13 are mended
Fill light needed for ccd image harvester 10, ccd image harvester 10 the etching state of sample is carried out acquisition in real time and into
Picture, 10 collected realtime graphic of ccd image harvester can be shown in display device or display module 7, as the present apparatus is shown
Image display program in computer.Wherein, adjust accurate burnt spiral 14, can focusedimage, make imaging clearly.Adjust camera lens
15 adjustable variable times camera lens 9 of object lens zoom knob, for changing the enlargement ratio of image.
The electrochemical etching unit includes power supply 17, and power supply 17 uses Digital DC Voltage-stabilized Power Source, further includes rectangular
Copper conductive electrode 18, the platinum filament coil 19 of body shape.19 first end of platinum filament coil connection copper conductive electrode 18,19 second end of platinum filament coil
Cyclic structure diameter is about 3mm.During work, the fixed specimen holder gripping member 20 of 17 anode of power supply connection, fixed specimen holder gripping member 20 is pressed from both sides
Sample 21 to be processed is held, the present apparatus is used as fixed specimen holder gripping member 20, power supply using low cost and practical metal tweezers at present
17 cathode connect copper conductive electrode 18, the electrolyte coated by the cyclic structure of 19 second end of platinum filament coil treat processed sample 21 into
Row localized etching.
The motorized precision translation stage 1 and copper conductive electrode 18 are fixed on pedestal 11, and position is adjustable, to be processed to ensure
Region is located at the central region of the real time monitoring unit.
Whole device flexibly changing etches position and lithographic method to meet the requirement of processing different shape sample.When need
When preparing microtrabeculae in sample end, by 300 × 300 μm of well cutting2The fixed specimen holder gripping member 20 of bar samples is clamped,
And it is placed between the upper clamp plate 4 of 1 top of motorized precision translation stage, lower clamp plate 5 and locks together.The position of motorized precision translation stage 1 is adjusted, makes to treat
Processed sample 21 is located at immediately below the camera lens of real time monitoring unit.Electrolyte on gently being dripped in platinum filament coil 19, makes in coil
Viscous last layer electrolyte membrane.It is translated by control module 6, sample 21 to be processed is slowly inserted perpendicularly into platinum filament coil 19
The cyclic structure center at two ends makes 21 front end of sample to be processed be covered by electrolyte membrane.Digital DC Voltage-stabilized Power Source is opened, from 0V
Gradually increase voltage, until bubble is uniformly emerged in electrolyte.Sample 21 to be processed is controlled in 10 μ ms by control module 6
Interior reciprocating movement makes the forward terminal of sample 21 to be processed uniformly etch, and replaces electrolyte in due course and repeats top-operation
Microtrabeculae is prepared in 21 end of sample to be processed.
When needing to prepare nanometer CT original position stretching samples, sample should be met in dog bone shape, make gauge length section again
Size reaches a nanometer CT sample sizes requirement, it is therefore desirable to by control module 6 apart from 200 μm of 21 end of a sample to be processed left side
Right position localized etching according to the method described above, until observing that etching spot size reaches requirement on display module 7
Stop.
Illustrate the process for using of described device with reference to embodiment.
Dog bone shape fine copper/pure nickel X ray nanometer CT in-situ mechanicals test micro-test sample is prepared, idiographic flow is：
(1) it using pure copper sheet/pure nickel piece of 500 μm or so of electric spark wire cutting machine cutting thickness, and is ground with sand paper
It is as thin as 300 μm.The buttress shaft that about 300 μm of width is cut into from copper sheet/nickel sheet is sawed using diamond wire saw.Flash trimming is removed using sand paper
Angle burr slightly polishes on surface.
(2) thin copper post is clamped with tweezers, and is placed between the upper clamp plate 4 of 1 top of motorized precision translation stage, lower clamp plate 5 and locks together
Tightly.The position of motorized precision translation stage 1 is adjusted, thin copper/nickel column is made to be located at immediately below the camera lens of real time monitoring unit, and make area to be etched
Domain is located at 7 center of display module.Adjusting accurate burnt spiral 14 and object lens zoom knob 15 makes imaging clearly.
(3) last layer electrolyte is gently dripped in the cyclic structure of 19 second end of platinum filament coil, cyclic structure is made to be stained with one
Layer electrolyte membrane.Sample is slowly inserted by hub of a spool by control module 6, it is just electrolyte membrane institute to make interested region
Covering.Slight adjustment coil angle, makes coil vertical with specimen cross section.The thin copper of confirmatory sample/nickel column and platinum filament coil be not mutual
Contact.Wherein the electrolyte of fine copper is matched by ethyl alcohol 125mL, distilled water 250mL, phosphatase 11 25mL, isopropanol 25mL, urea 2.5g
System；The electrolyte of pure nickel presses 7 by phosphoric acid and water:1 ratio is prepared.
(4) numerical control direct current voltage source 17 of electrochemical etching unit is opened, gradually enhances voltage from 0V, in real time observation electrolysis
Bubble is emerged rate and uniformity in liquid, until rate stabilization, stops pressurization when uniformity is preferable.Different materials are applicable in voltage not
Together, it need to repeatedly attempt.It is 2.5V such as fine copper, it is convenient for 3.0V for pure nickel.
(5) when finding that the deposit that is electrolysed out is excessive, to stop etching in time, and pass through control module 6 exit thin copper/
Nickel column, and dip the residue in alcohol cleaning coil with dropper.
(6) above (3)-(5) are repeated, until etch areas reaches required body diameter.
(7) in implementation process, it can realize that sample moves back and forth in a certain range by control module 6 simultaneously, make etching
Region is more uniformly distributed.
The fine copper micro-test sample prepared using development device is in kind as shown in Fig. 2, the diameter of most thin portion point is about 35.6 μm,
Meet size requirements of the X ray nanometer CT to fine copper sample.
The pure nickel micro-test sample prepared using development device is in kind as shown in figure 3, the diameter of most thin portion point is about 38.5 μm,
Meet size requirements of the X ray nanometer CT to pure nickel sample.
Claims (3)
1. the device for preparing X ray nanometer CT metal micro-test samples based on local electrochemical etching, which is characterized in that including precision
Position control unit, electrochemical etching unit, real time monitoring unit, the precise position control unit are used for the translation of sample；
The electrochemical etching unit is used for accurate etching sample, obtains required structure；The real time monitoring unit is for real-time
The etching state of sample is observed, and the state is acquired imaging；Wherein, precise position control unit includes uniaxial strip
There is spherical guide（8）Motorized precision translation stage（1）, stepping motor（2）, fixed specimen holder gripping member（20）Upper clamp plate（4）, lower folder
Plate（5）And control motorized precision translation stage（1）The control module of rate travel and its distance（6）, stepping motor（2）Drive electricity
Dynamic translation stage（1）It is mobile, upper clamp plate（4）, lower clamp plate（5）It is fixed on motorized precision translation stage（1）On；The power supply of electrochemical etching unit
（17）Using Digital DC Voltage-stabilized Power Source, power supply（17）Cathode connects copper conductive electrode（18）, power supply（17）The fixed sample of anode connection
Product clamping piece（20）；Unit is monitored in real time to include setting zoomable camera lens（9）Ccd image harvester（10）, fixing bracket
（12）, LED annular light sources（13）, adjust accurate burnt spiral（14）, wherein, ccd image harvester（10）It is fixed on fixing bracket
（12）On, by being arranged on fixing bracket（12）On the accurate burnt spiral of adjusting（14）Drive ccd image harvester（10）Longitudinal direction
Translation, LED annular light sources（13）Supplement ccd image harvester（10）Required light, ccd image harvester（10）To sample
Etching state acquired and be imaged in real time.
2. device as described in claim 1, which is characterized in that copper conductive electrode（18）Connect platinum filament coil（19）First end, platinum
Wire coil（19）Second end is arranged to cyclic structure, and coats electrolyte, copper conductive electrode（18）For block, it is placed on pedestal（11）
On.
3. device as described in claim 1, which is characterized in that ccd image harvester（10）Connect display device or display
Module（7）.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201721150007.7U CN207528521U (en) | 2017-09-08 | 2017-09-08 | The device for preparing X ray nanometer CT metal micro-test samples based on local electrochemical etching |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201721150007.7U CN207528521U (en) | 2017-09-08 | 2017-09-08 | The device for preparing X ray nanometer CT metal micro-test samples based on local electrochemical etching |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113186588A (en) * | 2021-04-06 | 2021-07-30 | 南京理工大学 | Automatic intelligent polishing equipment for preparing metal nanometer needle point sample |
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2017
- 2017-09-08 CN CN201721150007.7U patent/CN207528521U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113186588A (en) * | 2021-04-06 | 2021-07-30 | 南京理工大学 | Automatic intelligent polishing equipment for preparing metal nanometer needle point sample |
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Granted publication date: 20180622 Termination date: 20210908 |