CN107192660A - It is a kind of to be used for the apparatus and method that dynamic observes Cdl-x_Znx_Te chemical attack hole - Google Patents
It is a kind of to be used for the apparatus and method that dynamic observes Cdl-x_Znx_Te chemical attack hole Download PDFInfo
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Abstract
It is used for the apparatus and method that dynamic observes Cdl-x_Znx_Te chemical attack hole the invention discloses a kind of, 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, by the way that automatic feed liquor unit realizes being automatically injected of one or more corrosive liquids and cleaning fluid, dynamic updates and order switches, during the waste liquid that produces reclaimed immediately by devil liquor recovery unit, observation measurement and control unit is integrated with microscope, CCD camera, TT＆C software and storage device, carries out Real Time Observation, collection, display to the microprocess of material corrosion and stores.The present invention 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 improving corrosive effect.
Description
Technical field
The present invention relates to testing of materials manufacture field, refer specifically to a kind of dynamic that is used for and observe Cdl-x_Znx_Te chemical attack hole
Apparatus and method.
Background technology
CdZnTe can be realized and complete matching of the HgCdTe materials on lattice by composition regulation, be 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, and 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 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 and blind element rate of detector, 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 CdZnTe quality of materials most common methods, and it can disclose all kinds of in crystal well
Defect, has 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 can be because of preferential etch at corrosion certain time, 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：One be CdZnTe materials etch pit species it is a lot, structure and production to its corresponding defect
The research of life reason lacks effective means；Two be that the etch-pit density that various corrosive agent are produced has significant difference, different rotten
Corresponding relation between the etch pit that erosion agent is produced 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 formation microprocess and the difference on Forming Mechanism
It is different；(2) correlation that can not be between the etch pit of the different corrosive liquid formation of position observation；(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, Real Time Observation and the control realized in chemical corrosion process is specifically included, realized
The etching characteristic for observing all kinds of defects is accurately positioned, realizes that the dynamic of corrosive liquid updates and switched.
The content of the invention
The invention aims to provide a kind of dynamic that is used for observe device and the side that Cdl-x_Znx_Te chemical attack is cheated
Method, while solving deficiency of the existing chemical corrosion method in terms of process controllability, continuity, stability, and is research tellurium zinc
The structure of cadmium defect discloses effect with mechanism of production and the defect of the different corrosive liquids of evaluation and provides effective means.
It is used for the apparatus and method that dynamic observes Cdl-x_Znx_Te chemical attack hole the invention discloses a kind of, 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 the waste liquid that produces 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 is carried out to the microprocess of material corrosion, gathers, show and deposits
Storage.
The above-mentioned purpose of the present invention is achieved through the following technical solutions：
It is a kind of to be used for the device that dynamic observes 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 are constituted, it is characterised in that：The sample etches unit 1 by etching tank 1-1,
Main feed tube 1-2, corrosive liquid point feed tube 1-3, corrosive liquid liquid feed valve 1-4, cleaning fluid point 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 constitute, each liquid feeding pump two 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 is arrived at 50 times
Adjustable between 1000 times, observation measurement and control unit 4 can be cheated to material corrosion and produced and evolution process and fault in material and corrosive liquid
The characteristic of effect observed and record with dynamic in real time.
Sample is fixed in etching tank 1-1, transparent groove lid 1-10 is covered, selects to treat the area of corrosion observation using microscope
Corrosive liquid, is injected into etching tank 1-1 and sample is corroded by domain by corrosive liquid liquid feeding pump 2-2, starts positive displacement pump 3-2,
Corrosive liquid in corrosion process in etching tank 1-1 constantly alternately updates, while the waste liquid produced is collected into waste liquid tank 3-1 immediately
In, by microscope and CCD camera, dynamically observation and recording materials etch pit form evolving state in corrosion process, and 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 on the right side of the irregular cell body with certain depth, cell body
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
Divide the liquid feed valve for being fitted with individually controlling on feed tube 1-3 and cleaning fluid point feed tube 1-5, every point of feed tube, including corruption
Liquid liquid feed valve 1-4 and cleaning fluid liquid feed valve 1-6 is lost, is controlled respectively on the left of the feed liquor of a variety of corrosive liquids and cleaning fluid, etching tank 1-1
Bottom connected drainage pipe 1-7, discharge opeing pipe orifice is 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, available for optical observation, and 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
Groove lid 1-10 and etching tank 1-1 is sealed and fixed by 1-9；Etching tank 1-1 is that can carry out the sealing cell body of microexamination, internal corrosion
Liquid and its escaping gas are without leakage, while being connected to a variety of corrosive liquids and cleaning fluid.
It is a kind of to be used for the method that dynamic observes Cdl-x_Znx_Te chemical attack hole, it is characterised in that to comprise the following steps：
(1) by sample cutting-up into appropriate size, make sample surfaces that light as minute surface is presented after grinding and polishing；
(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 is dried 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, then cleaned 3 times or more with deionized water in methanol, 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, is poured into cleaning fluid fluid reservoir 2-3, is 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, the suitable amplification of selection
Multiple, regulation focuses on nut and sample upper surface is focused, and observes sample defects distribution situation, selects to treat the area of corrosion observation
Domain；
(7) by the corrosive liquid of etching tank point feed tube 1-3, cleaning fluid point 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, corresponding liquid feed valve 1-4 is opened, 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 starts fluid injection, is totally submerged after corrosive liquid after after corrosion sample, runs positive displacement pump 3-
2 start in discharge opeing, 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, and regulation positive displacement pump 3-2 flow velocitys to matching, operation cleaning fluid liquid feeding pump 2-4 starts injection cleaning
Liquid, until sample clean is clean, closes cleaning fluid liquid feeding pump 2-4 and liquid feed valve 1-6, treats that liquid is drained in etching tank 1-1, close
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) by remaining chemical corrosion liquid, cleaning fluid and the chemical waste fluid progress classification recovery reclaimed, deionization is used
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 and statistical analysis.
The present invention 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) feature is strong, in situ under fixed microscopic field of view can complete multistep corrosion cleaning, 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 1 sample etches unit in apparatus of the present invention flow chart, figure；1-1 etching tanks；The main feed tubes of 1-2；1-3 corrodes
Liquid point feed tube；1-4 corrosive liquid liquid feed valves；1-5 cleaning fluid point feed tubes；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 1-1 etching tanks in the structural representation of sample etches unit, 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 fluid point feed tubes；1-6 cleaning fluid liquid feed valves；1-7 discharging tubes；1-8 tapping valves；1-
9 sealing rings；1-10 groove lids.
Embodiment
The present invention is further elaborated below by instantiation, but the preferred embodiment that the present invention is provided, only it is used for
The present invention is illustrated, without being imposed any restrictions to the scope of the present invention, any one skilled in the art can be real easily
Existing modifications and variations are included in the present invention and scope of the following claims.
Embodiment 1：
(1) take along (211) face process cadmium zinc telluride crystal wafer, cutting-up into 20mm X 30mm, thickness be 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, makes sample surfaces that light as minute surface is presented；
(2) the trichloro ethylene cleaning sample of use boiling 3 times, reuse methanol cleaning sample 3 times, use 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 compares 100:20:5 prepare Everson corrosive liquids, stir, will prepare
Good Everson corrosive liquids are poured into corrosive liquid fluid reservoir 2-1, be 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) microscope light source is opened, sample etches groove 1-1 is placed on microscope example bench, selection multiplication factor is
100 times, regulation focuses on nut and sample upper surface is focused, and switches different microscope observing pattern observation sample defects point
Cloth situation, selects to treat the region of corrosion observation；
(7) by the corrosive liquid of etching tank point feed tube 1-3, cleaning fluid point feed tube 1-5 respectively with automatic feed liquor unit phase
Connection, the discharging tube 1-7 in left side is connected with positive displacement pump 3-2, confirms that the corrosive liquid liquid feed valve 1-4 of not connected feed liquor unit is in
Closed mode, confirms that cleaning fluid liquid feed valve 1-6 and tapping valve 1-8 is closed；
(8) set and control the liquid feeding pump 2-2 flow velocitys of Everson corrosive liquids for 6ml/min, open corresponding liquid feed valve 1-4, if
Positive displacement pump 3-2 flow velocitys are put for 6ml/min, tapping valve 1-8 is opened, operation liquid feeding pump 2-2 starts fluid injection, treats that corrosive liquid is totally submerged
After after corrosion sample, 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, the change procedure of etch pit is shown by CCD camera over the display, and image and video are gathered in real time, preserves number
According to；
(10) etching time is reached after 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, rinse after sample 3min, close cleaning fluid liquid feeding pump 2-4 and liquid feed valve 1-6, treat 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) by remaining chemical corrosion liquid, cleaning fluid and the chemical waste fluid progress classification recovery reclaimed, deionization is used
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 and statistical analysis.
Embodiment 2：
(1) take along (111) face process cadmium zinc telluride crystal wafer, cutting-up into 20mm X 20mm, thickness be 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, makes sample surfaces that light as minute surface is presented；
(2) the trichloro ethylene cleaning sample of use boiling 3 times, reuse methanol cleaning sample 3 times, use 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) 2 are compared by water, hydrogen peroxide, hydrofluoric acid volume: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) microscope light source is opened, sample etches groove 1-1 is placed on microscope example bench, selection multiplication factor is
200 times, regulation focuses on nut and sample upper surface is focused, and switches different microscope observing pattern observation sample defects point
Cloth situation, selects to treat the region of corrosion observation；
(7) by the corrosive liquid of etching tank point feed tube (1-3), cleaning fluid point 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) set and control the liquid feeding pump 2-2 flow velocitys of Nakagawa corrosive liquids for 4ml/min, open 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 after corrosion sample, 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, the change procedure of etch pit is shown by CCD camera over the display, and image and video are gathered in real time, preserves number
According to；
(10) etching time is reached after 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, rinse after sample 2min, close cleaning fluid liquid feeding pump 2-4 and liquid feed valve 1-6, treat 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) set and control the liquid feeding pump 2-2 flow velocitys of EAg-1 corrosive liquids for 5ml/min, open corresponding liquid feed valve 1-4, if
Positive displacement pump 3-2 flow velocitys are put for 5ml/min, tapping valve 1-8 is opened, operation liquid feeding pump 2-2 starts fluid injection, treats that corrosive liquid is totally submerged
After after corrosion sample, 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, the change procedure of etch pit is shown by CCD camera over the display, and image and video are gathered in real time, is preserved
Data；
(13) etching time is reached after 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 are arrived
25ml/min, is rinsed after sample 3min, is closed cleaning fluid liquid feeding pump 2-4 and liquid feed valve 1-6, is treated that liquid is drained in etching tank 1-1,
Close positive displacement pump 3-2 and tapping valve 1-8；
(14) by remaining chemical corrosion liquid, cleaning fluid and the chemical waste fluid progress classification recovery reclaimed, deionization is used
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 and statistical analysis.
Claims (3)
1. a kind of be used for the device that dynamic observes 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) is by etching tank (1-1), main feed tube (1-2), corrosive liquid point feed tube (1-3), corrosive liquid
It is liquid feed valve (1-4), cleaning fluid point 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) is by point feed tube (1-3,1-5) and automatically
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 two 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 in positive displacement pump (3-2), corrosion process and is corroded
Corrosive liquid in groove (1-1) constantly alternately updates, while the waste liquid produced is collected into waste liquid tank (3-1) immediately, corrodes
By microscope and CCD camera, dynamically observation and recording materials etch pit form evolving state 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 dynamic that is used for according to claim 1 observes the device that Cdl-x_Znx_Te chemical attack is cheated, its feature exists
In：The etching tank (1-1) is prepared by resistant material, is shaped as connecting on the right side of the irregular cell body with certain depth, cell body
Main feed tube (1-2) is connect, main feed liquor pipe orifice is communicated with the inside of etching tank (1-1), by main feed tube (1-2) if separating dry rot
Lose the feed liquor for being fitted with individually controlling on liquid point feed tube (1-3) and cleaning fluid point feed tube (1-5), every point of feed tube
Valve, including corrosive liquid liquid feed valve (1-4) and cleaning fluid liquid feed valve (1-6), control the feed liquor of a variety of corrosive liquids and cleaning fluid respectively,
Etching tank (1-1) left lower connected drainage pipe (1-7), discharge opeing pipe orifice is communicated 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 corrosion-resistant between etching tank (1-1) and groove lid (1-10)
Sealing ring (1-9), fixing screws be installed simultaneously sealed groove lid (1-10) and etching tank (1-1) by sealing ring (1-9) and fixed；
Etching tank (1-1) is can carry out the sealing cell body of microexamination, and internal corrosion liquid and its escaping gas are connected simultaneously without leakage
A variety of corrosive liquids and cleaning fluid.
3. a kind of observe the device that Cdl-x_Znx_Te chemical attack is cheated based on a kind of dynamic that is used for according to claim 1
The method in dynamic observation Cdl-x_Znx_Te chemical attack hole, it is characterised in that comprise the following steps：
1) by sample cutting-up into appropriate size, make sample surfaces that light as minute surface is presented after grinding and polishing；
2) using trichloro ethylene cleaning sample 3 times of boiling or more, methanol cleaning sample 3 times or more is reused, with high-purity
Nitrogen is dried 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 methanol
Cleaning 3 times or more, 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) center up, sample is carried out using Corrosion resistant adhesive tape to be bonded admittedly
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, is poured into cleaning fluid fluid reservoir (2-3), is 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, suitable times magnification is selected
Number, regulation focuses on nut and sample upper surface is focused, and observes sample defects distribution situation, selects to treat the area of corrosion observation
Domain；
7) by the corrosive liquid of etching tank point feed tube (1-3), cleaning fluid point 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
The corrosive liquid liquid feed valve (1-4) of feed liquor unit is closed, and confirms cleaning fluid liquid feed valve (1-6) and tapping valve (1-8) place
In closed mode；
8) corrosive liquid liquid feeding pump (2-2) flow velocity is set, corresponding liquid feed valve (1-4) is opened, positive displacement pump (3-2) flow velocity is set, is opened
Tapping valve (1-8), operation corrosive liquid liquid feeding pump (2-2) starts fluid injection, is totally submerged after corrosive liquid after after corrosion sample, operation is arranged
Liquid pump (3-2) starts in discharge opeing, corrosion process, sample is constantly in submerged state；
9) microscope focus is suitably finely tuned, microscope is clearly observed sample surfaces all the time, existed by CCD camera
The change procedure of etch pit is shown on display, image and video are gathered in real time, data are preserved；
10) after corrosion terminates, corrosive liquid liquid feeding pump (2-2) and liquid feed valve (1-4) are closed, cleaning fluid liquid feeding pump (2-4) stream is set
Speed, opens corresponding liquid feed valve (1-6), and regulation positive displacement pump (3-2) flow velocity to matching, operation cleaning fluid liquid feeding pump (2-4) starts note
Enter cleaning fluid, until sample clean is clean, closes cleaning fluid liquid feeding pump (2-4) and liquid feed valve (1-6), treat in etching tank (1-1)
Liquid is drained, and closes positive displacement pump (3-2) and tapping valve (1-8)；
11) if desired plurality of reagents is corroded or cleaned successively, repeat step 8) arrive step 10)；
12) by remaining chemical corrosion liquid, cleaning fluid and the chemical waste fluid progress classification recovery reclaimed, cleaned using deionized water
Related experiment utensil, drying；
13) sample surfaces are dried up using high pure nitrogen, the etch pit pattern of sample surfaces observed simultaneously using microscope
Statistical analysis.
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Cited By (3)
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|---|---|---|---|---|
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| CN110530786A (en) * | 2019-09-05 | 2019-12-03 | 北京科技大学 | A kind of device of in-situ observation steel surface local corrosion germinating process |
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| CN110186900A (en) * | 2019-06-11 | 2019-08-30 | 中国石油大学(华东) | A kind of test pond and its design method of the test metal erosion of coupling Raman spectrum |
| CN110530786A (en) * | 2019-09-05 | 2019-12-03 | 北京科技大学 | A kind of device of in-situ observation steel surface local corrosion germinating process |
| CN116908654A (en) * | 2023-07-24 | 2023-10-20 | 扬州国宇电子有限公司 | Automatic corrosion uncapping device for semiconductor packaging device |
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