CN207007672U - A kind of device for being used to dynamically observe Cdl-x_Znx_Te chemical attack hole - Google Patents
A kind of device for being used to dynamically observe Cdl-x_Znx_Te chemical attack hole Download PDFInfo
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- CN207007672U CN207007672U CN201720603943.2U CN201720603943U CN207007672U CN 207007672 U CN207007672 U CN 207007672U CN 201720603943 U CN201720603943 U CN 201720603943U CN 207007672 U CN207007672 U CN 207007672U
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Abstract
This patent discloses a kind of device for being used to dynamically observe Cdl-x_Znx_Te chemical attack hole, device is made up of sample etches unit, automatic feed liquor unit, devil liquor recovery unit and observation measurement and control unit.Sample is fixed in the etching tank that can carry out optical observation, being automatically injected, dynamically update and sequentially switching for one or more corrosive liquids and cleaning fluid is realized by automatic feed liquor unit, during caused waste liquid reclaimed immediately by devil liquor recovery unit, observation measurement and control unit is integrated with microscope, CCD camera, TT＆C software and storage device, and Real Time Observation, collection, display and storage are carried out to the microprocess of material corrosion.This patent can Real Time Observation recording materials etch pit from produce to disappearance dynamic process, in situ under fixed microscopic field of view it can complete multistep corrosion cleaning, the dynamic renewal of corrosive liquid in corrosion process can be realized, controllability, the stability of technique are effectively increased, while improves corrosive effect.
Description
Technical field
This patent is related to testing of materials manufacture field, refers specifically to a kind of for dynamically observing Cdl-x_Znx_Te chemical attack hole
Device.
Background technology
CdZnTe can be realized by composition regulation and complete matching of the HgCdTe materials on lattice, is to prepare low dislocation
The preferred substrate of density HgCdTe epitaxial materials, CdZnTe base HgCdTe epitaxial materials are in high-performance, long wave, very long wave, APD etc.
Third generation HgCdTe infrared detectors field plays important role.In addition, CdZnTe can also be used to prepare solar cell
And gamma ray detector, CdTe solar cells have occupied half of the country in solar power station field, γ prepared by CdZnTe is visited
Device is surveyed to have a wide range of applications in fields such as Aid of Space Remote Sensing Technology, safety check technology, medical diagnosis technology and weaponrys.
CdZnTe materials have that growth temperature is high, thermal conductivity is low, heap barrier layer is wrong compared with the semi-conducting materials such as Si and GaAs
Energy is low, component easily many unfavorable factors such as fractional condensation, in addition, it was found from Cd-Te system phasors, CdZnTe materials can be sent out at high temperature
Biochemical proportioning deviates, and easily produces various be mingled with and sediment.Therefore, compared with Si and GaAs semi-conducting materials, CdZnTe
Many tiny flaws are constantly present in material, are mainly answered including dislocation, sediment, field trash, fault, twin, crystal boundary, part
Power etc..The presence of these defects can directly affect quality of materials, so as to influence the uniformity of detector and blind element rate, reduce device
Performance even results in component failure, therefore intuitively and accurately evaluates the quality of CdZnTe materials and further investigate all kinds of defects
Characteristic tool is of great significance.
Chemical corrosion method is to evaluate the most frequently used method of CdZnTe quality of materials, and it can disclose all kinds of in crystal well
Defect, have the advantages that easy to operate, cost is low and sample is easily prepared.The chemical corrosion liquid of certain volume is first prepared, will be passed through
CdZnTe materials after grinding and polishing are put into corrosion certain time, can be because of preferential etch at material existing defects or local stress
And pit is formed, material is taken out and cleaned up, the quality of crystal is judged by the density of statistical material surface chemistry etch pit.
Common CdZnTe crystal corrosive agent has Inoue (EAg-1, EAg-2), Nagakawa and Everson corrosive agent.Prior art
Problem of both being primarily present：First, the etch pit species of CdZnTe materials is a lot, structure and production to its corresponding defect
The research of life reason lacks effective means；Second, significant difference be present in etch-pit density caused by various corrosive agent, it is different rotten
Corresponding relation between etch pit caused by erosion agent is difficult to be confirmed from experiment.The reason for producing these problems is existing
Chemical corrosion method has the following disadvantages：(1) can not position observation etch pit formed microprocess and the difference on Forming Mechanism
It is different；(2) can not position observation difference corrosive liquid formed etch pit between correlation；(3) existing caustic solution is not active
State updates corrosive liquid, causes etching condition unstable, technology stability is poor.In summary, existing CdZnTe chemistry is improved
The problem of etch quality evaluation technology, core was to improve the controllability of technique, stability, and chemically corroded
The more information of fault in material is obtained in technology, specifically includes Real Time Observation and the control realized in chemical corrosion process, is realized
The etching characteristic for observing all kinds of defects is accurately positioned, realizes the dynamic renewal and switching of corrosive liquid.
The content of the invention
The purpose of this patent is to provide for a kind of device for being used to dynamically observe Cdl-x_Znx_Te chemical attack hole, simultaneously
Solve deficiency of the existing chemical corrosion method in process controllability, continuity, stability etc., and be research cadmium-zinc-teiluride defect
The defects of structure and mechanism of production and evaluation different corrosive liquids, discloses effect and provides effective means.
This patent discloses a kind of apparatus and method for being used to dynamically observe Cdl-x_Znx_Te chemical attack hole, device is by sample
Product erosion unit, automatic feed liquor unit, devil liquor recovery unit and observation measurement and control unit composition.Sample, which is fixed on, can carry out optics
In the etching tank of observation, being automatically injected of one or more corrosive liquids and cleaning fluid, dynamic are realized more by automatic feed liquor unit
New and order switches, during caused waste liquid reclaimed immediately by devil liquor recovery unit, observation measurement and control unit be integrated with microscope,
CCD camera, TT＆C software and storage device, Real Time Observation, collection are carried out to the microprocess of material corrosion, shows and deposits
Storage.
The above-mentioned purpose of this patent is achieved through the following technical solutions：
A kind of device for being used to dynamically observe Cdl-x_Znx_Te chemical attack hole, by sample etches unit 1, automatic feed liquor list
Member 2, devil liquor recovery unit 3 and observation measurement and control unit 4 form, it is characterised in that：The sample etches unit 1 by etching tank 1-1,
Main feed tube 1-2, corrosive liquid divide feed tube 1-3, corrosive liquid liquid feed valve 1-4, cleaning fluid to divide feed tube 1-5, cleaning fluid liquid feed valve
1-6, discharging tube 1-7, tapping valve 1-8, sealing ring 1-9, groove lid 1-10 and fixing screws composition, sample etches unit 1 is by dividing
Feed tube 1-3,1-5 are connected with automatic feed liquor unit 2, and sample etches unit 1 passes through discharging tube 1-7 and devil liquor recovery unit 3
It is connected；The automatic feed liquor unit 2 by corrosive liquid fluid reservoir 2-1, corrosive liquid liquid feeding pump 2-2, cleaning fluid fluid reservoir 2-3 and
Cleaning fluid liquid feeding pump 2-4 form, each liquid feeding pump both ends by flexible pipe respectively with fluid reservoir a 2-1,2-3 and a point of feed liquor
Pipe 1-3,1-5 are connected, and starting automatic feed liquor unit 2 can be automatically by fluid reservoir 2-1, and corrosive liquid and cleaning fluid in 2-3 are simultaneously
Or it is sequentially injected into etching tank 1-1；The devil liquor recovery unit 3 is made up of waste liquid tank 3-1 and positive displacement pump 3-2, and positive displacement pump 3-2 leads to
Cross flexible pipe respectively with waste liquid tank 3-1 and discharging tube 1-7 to be connected, starting devil liquor recovery unit 3 can be by the liquid in etching tank 1-1
Automatically it is discharged into waste liquid tank 3-1；The observation measurement and control unit 4 is made up of microscope, CCD camera, TT＆C software and storage device,
Wherein microscopical observing pattern can switch between visible reflectance and infrared transmission, and overall multiplication factor arrives at 50 times
Adjustable between 1000 times, observation measurement and control unit 4 can cheat generation and evolution process and fault in material and corrosive liquid to material corrosion
The characteristic of effect is carried out in real time and dynamic is observed and record.
Sample is fixed in etching tank 1-1, covers transparent groove lid 1-10, selects to treat the area of corrosion observation using microscope
Domain, corrosive liquid is injected into etching tank 1-1 by corrosive liquid liquid feeding pump 2-2 sample is corroded, start positive displacement pump 3-2,
Corrosive liquid in corrosion process in etching tank 1-1 is constantly alternately updated, and waste liquid tank 3-1 is collected into immediately with caused waste liquid
In, evolving state is formed by microscope and the observation of CCD camera dynamic and recording materials etch pit in corrosion process, corrosion terminates
Afterwards, cleaning fluid is injected into etching tank 1-1 by cleaning fluid liquid feeding pump 2-4, until sample is cleaned.
The etching tank 1-1 is prepared by resistant material, is shaped as the irregular cell body with certain depth, cell body right side
Main feed tube 1-2 is connected, main feed liquor pipe orifice is communicated with etching tank 1-1 inside, and some corrosive liquids are separated by main feed tube 1-2
Feed tube 1-3 is divided to divide feed tube 1-5 with cleaning fluid, every is divided on feed tube the liquid feed valve for being fitted with individually controlling, including corruption
Liquid liquid feed valve 1-4 and cleaning fluid liquid feed valve 1-6 is lost, controls the feed liquor of a variety of corrosive liquids and cleaning fluid, etching tank 1-1 left sides respectively
Bottom connected drainage pipe 1-7, discharge opeing pipe orifice are communicated with etching tank 1-1 inside, and tapping valve 1-8 is provided with discharging tube 1-7；
Etching tank 1-1 upper surfaces surrounding has screwed hole some, for installing fixing screws；Groove lid 1-10 and etching tank 1-1 upper surfaces shape
Shape size is identical, and material is transparent material, and available for optical observation, surrounding has through hole some and etching tank 1-1 upper surfaces screw thread
Hole is corresponding, and corrosion resistant sealing ring 1-9 is set between etching tank 1-1 and groove lid 1-10, installs fixing screws and passes through sealing ring
1-9 fixes groove lid 1-10 and etching tank 1-1 sealings；Etching tank 1-1 is that can carry out the sealing cell body of microexamination, internal corrosion
Liquid and its escaping gas are connected to a variety of corrosive liquids and cleaning fluid without leakage.
A kind of method for being used to dynamically observe Cdl-x_Znx_Te chemical attack hole, it is characterised in that comprise the following steps：
(1) by sample cutting-up into appropriate size, present sample surfaces after grinding and polishing bright as minute surface；
(2) using trichloro ethylene cleaning sample 3 times of boiling or more, methanol cleaning sample 3 times or more is reused, is used
High pure nitrogen dries up；
(3) the bromine methanol solution that bromine volume fraction is 5 ‰ is prepared, sample is put into corrosion 15 seconds, is then quickly put into
Clean 3 times or more in methanol, then cleaned 3 times or more with deionized water, dried up with high pure nitrogen；
(4) sample is treated that corrosion is placed on etching tank 1-1 centers up, sample is bonded using Corrosion resistant adhesive tape
It is fixed, groove lid 1-10 is covered, is fixed using fixing screws；
(5) corrosive liquid needed for preparing is poured into corrosive liquid fluid reservoir 2-1, is connected with corrosive liquid liquid feeding pump 2-2, is prepared
Required cleaning fluid, pour into cleaning fluid fluid reservoir 2-3, be connected with cleaning fluid liquid feeding pump 2-4, waste liquid tank 3-1 and positive displacement pump
3-2 is connected；
(6) microscope light source is opened, sample etches groove 1-1 is placed on microscope example bench, selects suitable amplification
Multiple, regulation focus on nut and sample upper surface are focused, and observe sample defects distribution situation, select to treat the area of corrosion observation
Domain；
(7) by the corrosive liquid of etching tank divide feed tube 1-3, cleaning fluid divide feed tube 1-5 respectively with corrosive liquid liquid feeding pump 2-2
And cleaning fluid liquid feeding pump 2-4 is connected, the discharging tube 1-7 in left side is connected with positive displacement pump 3-2, confirms not connected feed liquor unit
Corrosive liquid liquid feed valve 1-4 be closed, confirm cleaning fluid liquid feed valve 1-6 and tapping valve 1-8 be closed；
(8) corrosive liquid liquid feeding pump 2-2 flow velocitys are set, open corresponding liquid feed valve 1-4, positive displacement pump 3-2 flow velocitys are set, the row of opening
Liquid valve 1-8, operation corrosive liquid liquid feeding pump 2-2 start fluid injection, are totally submerged after corrosive liquid after sample is corroded, operation positive displacement pump 3-
2 start discharge opeings, in corrosion process, sample is constantly in submerged state；
(9) microscope focus is suitably finely tuned, microscope is clearly observed sample surfaces all the time, pass through CCD
Camera shows the change procedure of etch pit over the display, and image and video are gathered in real time, preserves data；
(10) after corrosion terminates, corrosive liquid liquid feeding pump 2-2 and liquid feed valve 1-4 is closed, cleaning fluid liquid feeding pump 2-4 streams are set
Speed, opens corresponding liquid feed valve 1-6, regulation positive displacement pump 3-2 flow velocitys to matching, and operation cleaning fluid liquid feeding pump 2-4 starts injection cleaning
Liquid, until sample clean is clean, cleaning fluid liquid feeding pump 2-4 and liquid feed valve 1-6 is closed, treats that liquid drains in etching tank 1-1, closed
Positive displacement pump 3-2 and tapping valve 1-8；
(11) if desired plurality of reagents is corroded or cleaned successively, and repeat step (8) arrives step (10)；
(12) remaining chemical corrosion liquid, cleaning fluid and the chemical waste fluid of recovery are subjected to classification recovery, use deionization
Water cleans related experiment utensil, drying；
(13) sample surfaces are dried up using high pure nitrogen, the etch pit pattern of sample surfaces seen using microscope
Examine simultaneously statistical analysis.
This patent has the following advantages that：
(1) dynamic is directly perceived, being capable of dynamic process of the Real Time Observation recording materials etch pit from generation to disappearance；
(2) functional, in situ under fixed microscopic field of view multistep corrosion cleaning can be completed, various corrosive liquids are cut
Former chemical liquids will not be remained when changing in etching tank；
(3) stability is high, can realize the dynamic renewal of corrosive liquid in corrosion process, keep etch state stable；
(4) technological effect is good, and corrosion sample is not oxidizable.
Brief description of the drawings
Fig. 1 is patent device flow chart, 1 sample etches unit in figure；1-1 etching tanks；The main feed tubes of 1-2；1-3 corrodes
Liquid divides feed tube；1-4 corrosive liquid liquid feed valves；1-5 cleaning fluids divide feed tube；1-6 cleaning fluid liquid feed valves；1-7 discharging tubes；1-8 is arranged
Liquid valve；2 automatic feed liquor units；2-1 corrosive liquid fluid reservoirs；2-2 corrosive liquid liquid feeding pumps；2-3 cleaning fluid fluid reservoirs；2-4 cleaning fluids
Liquid feeding pump；3- devil liquor recovery units；3-1 waste liquid tanks；3-2 positive displacement pumps；4 observation measurement and control units.
Fig. 2 is the structural representation of sample etches unit, 1-1 etching tanks in figure；The main feed tubes of 1-2；1-3 corrosive liquids point enter
Liquid pipe；1-4 corrosive liquid liquid feed valves；1-5 cleaning fluids divide feed tube；1-6 cleaning fluid liquid feed valves；1-7 discharging tubes；1-8 tapping valves；1-
9 sealing rings；1-10 groove lids.
Embodiment
This patent is further elaborated below by instantiation, but the preferred embodiment that this patent provides, only it is used for
This patent is illustrated, without being imposed any restrictions to the scope of this patent, any one skilled in the art can be real easily
Existing modifications and variations are included in this patent and scope of the following claims.
Embodiment 1：
(1) take the cadmium zinc telluride crystal wafer along the processing of (211) face, cutting-up into 20mm X 30mm, thickness 1mm, sample
(211) B faces first remove 50 μm using the grinding of the 3 micrometer alumina aqueous solution, reuse Chemlox polishing fluids and carry out chemical machinery throwing
Light removes 20um, sample surfaces is presented bright as minute surface；
(2) the trichloro ethylene cleaning sample of use boiling 3 times, reuse methanol cleaning sample 3 times, with High Purity Nitrogen air-blowing
It is dry；
(3) the bromine methanol solution that bromine volume fraction is 5 ‰ is prepared, sample (211) B is put into corrosion 15 seconds up,
Then quickly it is put into methanol and cleans 3 times, then cleaned 3 times with deionized water, is dried up with high pure nitrogen；
(4) sample (211) B is placed on lower etching tank 1-1 centers up, sample glued using Corrosion resistant adhesive tape
Fixation is connect, groove lid 1-10 is covered, is fixed using fixing screws；
(5) lactic acid is pressed：Nitric acid：Hydrofluoric acid volume is than 100:20:5 prepare Everson corrosive liquids, stir, will prepare
Good Everson corrosive liquids are poured into corrosive liquid fluid reservoir 2-1, are connected with corrosive liquid liquid feeding pump 2-2, deionized water is poured into
In cleaning fluid fluid reservoir 2-3, and it is connected with cleaning fluid liquid feeding pump 2-4, waste liquid tank 3-1 is connected with positive displacement pump 3-2；
(6) open microscope light source, sample etches groove 1-1 is placed on microscope example bench, select multiplication factor for
100 times, regulation focuses on nut and sample upper surface is focused, and switches different microscope observing pattern observation sample defects point
Cloth situation, select to treat the region of corrosion observation；
(7) by the corrosive liquid of etching tank divide feed tube 1-3, cleaning fluid divide feed tube 1-5 respectively with automatic feed liquor unit phase
Connection, the discharging tube 1-7 in left side are connected with positive displacement pump 3-2, confirm that the corrosive liquid liquid feed valve 1-4 of not connected feed liquor unit is in
Closed mode, confirm that cleaning fluid liquid feed valve 1-6 and tapping valve 1-8 is closed；
(8) it is 6ml/min that setting, which controls the liquid feeding pump 2-2 flow velocitys of Everson corrosive liquids, opens corresponding liquid feed valve 1-4, if
It is 6ml/min to put positive displacement pump 3-2 flow velocitys, opens tapping valve 1-8, and operation liquid feeding pump 2-2 starts fluid injection, treats that corrosive liquid is totally submerged
After sample is corroded, operation positive displacement pump 3-2 starts discharge opeing, fine setting liquid feeding pump 2-2 and positive displacement pump 3-2 flow velocitys, maintains etching tank 1-1
The dynamic renewal of interior chemical corrosion liquid, and sample is constantly in submerged state；
(9) in corrosion process, microscope focus is suitably finely tuned, microscope is clearly observed sample table all the time
Face, show the change procedure of etch pit over the display by CCD camera, image and video are gathered in real time, preserve number
According to；
(10) after etching time reaches 150s, the liquid feeding pump 2-2 and liquid feed valve 1-4 of closing control Everson corrosive liquids, so
The liquid feeding pump 2-4 and liquid feed valve 1-6 of control deionized water are opened afterwards, and setting flow velocity is 30ml/min, adjusts positive displacement pump 3-2 flow velocitys
To 30ml/min, after rinsing sample 3min, cleaning fluid liquid feeding pump 2-4 and liquid feed valve 1-6 is closed, treats that liquid is arranged in etching tank 1-1
To the greatest extent, positive displacement pump 3-2 and tapping valve 1-8 is closed；
(11) remaining chemical corrosion liquid, cleaning fluid and the chemical waste fluid of recovery are subjected to classification recovery, use deionization
Water cleans related experiment utensil, drying；
(12) sample surfaces are dried up using high pure nitrogen, the etch pit pattern of sample surfaces seen using microscope
Examine simultaneously statistical analysis.
Embodiment 2：
(1) take the cadmium zinc telluride crystal wafer along the processing of (111) face, cutting-up into 20mm X 20mm, thickness 3mm, sample
(111) A faces first remove 30 μm using the grinding of the 3 micrometer alumina aqueous solution, reuse Chemlox polishing fluids and carry out chemical machinery throwing
Light removes 15um, sample surfaces is presented bright as minute surface；
(2) the trichloro ethylene cleaning sample of use boiling 3 times, reuse methanol cleaning sample 3 times, with High Purity Nitrogen air-blowing
It is dry；
(3) the bromine methanol solution that bromine volume fraction is 5 ‰ is prepared, sample (111) A is put into corrosion 15 seconds up,
Then quickly it is put into methanol and cleans 3 times, then cleaned 3 times with deionized water, is dried up with high pure nitrogen；
(4) sample (111) A is placed on lower etching tank 1-1 centers up, sample glued using Corrosion resistant adhesive tape
Fixation is connect, groove lid 1-10 is covered, is fixed using fixing screws；；
(5) by water, hydrogen peroxide, hydrofluoric acid volume than 2:2:3 prepare Nakagawa corrosive liquids, by nitric acid, water, potassium bichromate
Ratio is 10ml:10ml:4g prepares E solution, is 10ml according still further to E solution, silver nitrate ratio:0.5mg prepares EAg-1 corrosion
Liquid, Nakagawa corrosive liquids, EAg-1 corrosive liquids are poured into 2 corrosive liquid fluid reservoir 2-1 respectively, with corrosive liquid liquid feeding pump 2-2
It is connected, deionized water is poured into cleaning fluid fluid reservoir 2-3, and be connected with cleaning fluid liquid feeding pump 2-4, by waste liquid tank 3-1
It is connected with positive displacement pump 3-2；
(6) open microscope light source, sample etches groove 1-1 is placed on microscope example bench, select multiplication factor for
200 times, regulation focuses on nut and sample upper surface is focused, and switches different microscope observing pattern observation sample defects point
Cloth situation, select to treat the region of corrosion observation；
(7) by the corrosive liquid of etching tank divide feed tube (1-3), cleaning fluid divide feed tube 1-5 respectively with automatic feed liquor unit
It is connected, the discharging tube 1-7 in left side is connected with positive displacement pump 3-2, at the corrosive liquid liquid feed valve 1-4 for confirming not connected feed liquor unit
In closed mode, confirm that cleaning fluid liquid feed valve 1-6 and tapping valve 1-8 is closed；
(8) it is 4ml/min that setting, which controls the liquid feeding pump 2-2 flow velocitys of Nakagawa corrosive liquids, opens corresponding liquid feed valve 1-4,
It is 4ml/min to set positive displacement pump 3-2 flow velocitys, opens tapping valve 1-8, and operation liquid feeding pump 2-2 starts fluid injection, treats that corrosive liquid soaks completely
Not after sample is corroded, operation positive displacement pump 3-2 starts discharge opeing, fine setting liquid feeding pump 2-2 and positive displacement pump 3-2 flow velocitys, maintains etching tank
The dynamic renewal of chemical corrosion liquid in 1-1, and sample is constantly in submerged state；
(9) in corrosion process, microscope focus is suitably finely tuned, microscope is clearly observed sample table all the time
Face, show the change procedure of etch pit over the display by CCD camera, image and video are gathered in real time, preserve number
According to；
(10) after etching time reaches 45s, the liquid feeding pump 2-2 and liquid feed valve 1-4 of closing control Nakagawa corrosive liquids, so
The liquid feeding pump 2-4 and liquid feed valve 1-6 of control deionized water are opened afterwards, and setting flow velocity is 20ml/min, adjusts positive displacement pump 3-2 flow velocitys
To 20ml/min, after rinsing sample 2min, cleaning fluid liquid feeding pump 2-4 and liquid feed valve 1-6 is closed, treats that liquid is arranged in etching tank 1-1
To the greatest extent, positive displacement pump 3-2 and tapping valve 1-8 is closed；
(11) it is 5ml/min that setting, which controls the liquid feeding pump 2-2 flow velocitys of EAg-1 corrosive liquids, opens corresponding liquid feed valve 1-4, if
It is 5ml/min to put positive displacement pump 3-2 flow velocitys, opens tapping valve 1-8, and operation liquid feeding pump 2-2 starts fluid injection, treats that corrosive liquid is totally submerged
After sample is corroded, operation positive displacement pump 3-2 starts discharge opeing, fine setting liquid feeding pump 2-2 and positive displacement pump 3-2 flow velocitys, maintains etching tank 1-1
The dynamic renewal of interior chemical corrosion liquid, and sample is constantly in submerged state；
(12) in corrosion process, microscope focus is suitably finely tuned, microscope is clearly observed sample all the time
Surface, show the change procedure of etch pit over the display by CCD camera, image and video are gathered in real time, preserve
Data；
(13) after etching time reaches 30s, the liquid feeding pump 2-2 and liquid feed valve 1-4 of closing control EAg-1 corrosive liquids, then
The liquid feeding pump 2-4 and liquid feed valve 1-6 of control deionized water are opened, setting flow velocity is 25ml/min, and regulation positive displacement pump 3-2 flow velocitys arrive
25ml/min, after rinsing sample 3min, cleaning fluid liquid feeding pump 2-4 and liquid feed valve 1-6 is closed, treats that liquid drains in etching tank 1-1,
Close positive displacement pump 3-2 and tapping valve 1-8；
(14) remaining chemical corrosion liquid, cleaning fluid and the chemical waste fluid of recovery are subjected to classification recovery, use deionization
Water cleans related experiment utensil, drying；
(15) sample surfaces are dried up using high pure nitrogen, the etch pit pattern of sample surfaces seen using microscope
Examine simultaneously statistical analysis.
Claims (2)
- A kind of 1. device for being used to dynamically observe Cdl-x_Znx_Te chemical attack hole, by sample etches unit (1), automatic feed liquor list First (2), devil liquor recovery unit (3) and observation measurement and control unit (4) composition, it is characterised in that：The sample etches unit (1) divides feed tube (1-3), corrosive liquid by etching tank (1-1), main feed tube (1-2), corrosive liquid Liquid feed valve (1-4), cleaning fluid divide feed tube (1-5), cleaning fluid liquid feed valve (1-6), discharging tube (1-7), tapping valve (1-8), close Seal (1-9), groove lid (1-10) and fixing screws composition, sample etches unit (1) by divide feed tube (1-3,1-5) with it is automatic Feed liquor unit (2) is connected, and sample etches unit (1) is connected by discharging tube (1-7) with devil liquor recovery unit (3)；The automatic feed liquor unit (2) is by corrosive liquid fluid reservoir (2-1), corrosive liquid liquid feeding pump (2-2), cleaning fluid fluid reservoir (2- 3) and cleaning fluid liquid feeding pump (2-4) composition, each liquid feeding pump both ends by flexible pipe respectively with a fluid reservoir (2-1,2-3) and A piece point of feed tube (1-3,1-5) is connected, and starting automatic feed liquor unit (2) can be automatically by the corruption in fluid reservoir (2-1,2-3) Erosion liquid and cleaning fluid simultaneously or sequentially inject etching tank (1-1)；The devil liquor recovery unit (3) is made up of waste liquid tank (3-1) and positive displacement pump (3-2), and positive displacement pump (3-2) is distinguished by flexible pipe It is connected with waste liquid tank (3-1) and discharging tube (1-7), starting devil liquor recovery unit (3) can be by the liquid in etching tank (1-1) certainly It is dynamic to be discharged into waste liquid tank (3-1)；The observation measurement and control unit (4) is made up of microscope, CCD camera, TT＆C software and storage device, wherein microscopical Observing pattern switches between visible reflectance and infrared transmission, and overall multiplication factor is adjustable between 50 times to 1000 times；Sample is placed in etching tank (1-1), selects to treat the region of corrosion observation, to pass through corrosive liquid liquid feeding pump using microscope Corrosive liquid is injected into etching tank (1-1) by (2-2) to be corroded to sample, is started positive displacement pump (3-2), is corroded in corrosion process Corrosive liquid in groove (1-1) constantly alternately updates, and is collected into waste liquid tank (3-1), corroded immediately with caused waste liquid Evolving state is formed by microscope and the observation of CCD camera dynamic and recording materials etch pit in journey, after corrosion terminates, by clear Cleaning fluid is injected into etching tank (1-1) by washing lotion liquid feeding pump (2-4), until sample is cleaned.
- 2. a kind of device for being used to dynamically observe Cdl-x_Znx_Te chemical attack hole according to claim 1, its feature exist In：The etching tank (1-1) is prepared by resistant material, is shaped as the irregular cell body with certain depth, is connected on the right side of cell body Main feed tube (1-2) is connect, main feed liquor pipe orifice communicates with the inside of etching tank (1-1), by main feed tube (1-2) if separating dry rot Erosion liquid divides feed tube (1-3) to divide feed tube (1-5) with cleaning fluid, and every is divided on feed tube the feed liquor for being fitted with individually controlling Valve, including corrosive liquid liquid feed valve (1-4) and cleaning fluid liquid feed valve (1-6), the feed liquor of a variety of corrosive liquids and cleaning fluid is controlled respectively, Etching tank (1-1) left lower connected drainage pipe (1-7), discharge opeing pipe orifice communicate with the inside of etching tank (1-1), discharging tube Tapping valve (1-8) is installed on (1-7)；Etching tank (1-1) upper surface surrounding has screwed hole some, for installing fixing screws； Groove lid (1-10) is identical with etching tank (1-1) upper surface shape size, and material is transparent material, available for optical observation, surrounding There is through hole some corresponding with etching tank (1-1) upper surface screwed hole, set between etching tank (1-1) and groove lid (1-10) corrosion-resistant Sealing ring (1-9), installation fixing screws simultaneously by sealing ring (1-9) by groove lid (1-10) and etching tank (1-1) sealing fix； Etching tank (1-1) is the sealing cell body that can carry out microexamination, and internal corrosion liquid and its escaping gas connect simultaneously without leakage A variety of corrosive liquids and cleaning fluid.
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| CN113008650A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Metallographic corrosive agent and metallographic corrosive method for UN fuel pellets |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113008650A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Metallographic corrosive agent and metallographic corrosive method for UN fuel pellets |
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