CN107192660B - Device and method for dynamically observing tellurium-zinc-cadmium material chemical corrosion pits - Google Patents
Device and method for dynamically observing tellurium-zinc-cadmium material chemical corrosion pits Download PDFInfo
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Abstract
The invention discloses a device and a method for dynamically observing a tellurium-zinc-cadmium material chemical corrosion pit. The method comprises the steps of fixing a sample in an optical observable corrosion tank, automatically injecting one or more corrosive liquids and cleaning liquids through an automatic liquid inlet unit, dynamically updating and sequentially switching, and immediately recovering waste liquid generated in the process by a waste liquid recovery unit, wherein the observation and measurement unit integrates a microscope, a CCD camera, measurement and control software and storage equipment, and performs real-time observation, collection, display and storage on microscopic processes of material corrosion. The invention can observe the dynamic process from generation to disappearance of the corrosion pit of the recording material in real time, can complete the multi-step corrosion cleaning process in situ under a fixed microscopic view field, can realize the dynamic update of the corrosion liquid in the corrosion process, effectively improves the controllability, the continuity and the stability of the process, and improves the corrosion effect.
Description
Technical Field
The invention relates to the field of material testing and processing, in particular to a device and a method for dynamically observing a chemical corrosion pit of a tellurium-zinc-cadmium material.
Background
The CdZnTe can be completely matched with the HgCdTe material in crystal lattice through component adjustment, is a preferred substrate for preparing the HgCdTe epitaxial material with low dislocation density, and plays an important role in the fields of third-generation HgCdTe infrared detectors such as high performance, long wave, very long wave, APD and the like. In addition, the CdZnTe can be used for preparing solar cells and gamma ray detectors, the CdTe solar cells occupy the half-wall Jiangshan in the field of solar power stations, and the gamma detector prepared by the CdZnTe has wide application in the fields of space remote sensing technology, security inspection technology, medical diagnosis technology, weaponry and the like.
Compared with semiconductor materials such as Si, gaAs and the like, the CdZnTe material has the defects of high growth temperature, low heat conductivity, low stacking fault energy, easiness in component segregation and the like, and in addition, the CdZnTe material is subject to chemical proportion deviation at high temperature and is extremely easy to generate various impurities and precipitates as known from a Cd-Te system phase diagram. Therefore, many tiny defects are always present in CdZnTe materials, mainly including dislocations, precipitates, inclusions, faults, twins, grain boundaries, local stresses, etc., compared to Si and GaAs semiconductor materials. The existence of the defects can directly influence the quality of the material, thereby influencing the uniformity and blind pixel rate of the detector, reducing the performance of the device and even causing the failure of the device, so that the method has very important significance in intuitively and accurately evaluating the quality of the CdZnTe material and deeply researching the characteristics of various defects.
The chemical corrosion method is the most commonly used method for evaluating the quality of CdZnTe materials, can well reveal various defects in crystals, and has the advantages of simple operation, low cost, easy preparation of samples and the like. Preparing a certain volume of chemical etching liquid, putting the CdZnTe material subjected to grinding and polishing into the material to be etched for a certain time, forming pits at the positions where the material has defects or local stress due to preferential etching, taking out the material to clean, and judging the quality of crystals by counting the density of the chemical etching pits on the surface of the material. Common CdZnTe crystal etchants are Inoue (EAg-1, EAg-2), nagakawa, and Everson etchants. The prior art mainly has two problems: firstly, the corrosion pits of CdZnTe materials are various, and the research on the structure and the generation mechanism of the corresponding defects of the CdZnTe materials lacks effective means; secondly, the densities of corrosion pits generated by various corrosives are significantly different, and the correspondence between the corrosion pits generated by different corrosives is difficult to confirm from experiments. These problems are caused by the following disadvantages of the existing chemical etching methods: (1) The microscopic process of etch pit formation and the differences in the formation mechanisms cannot be located and observed; (2) The mutual relation between corrosion pits formed by different corrosive liquids cannot be positioned and observed; (3) The existing corrosion method can not dynamically update the corrosion liquid, so that the corrosion condition is unstable and the process stability is relatively poor. In summary, the core of the improvement of the existing CdZnTe chemical corrosion method quality evaluation technology is to improve the controllability, continuity and stability of the process, obtain more information of material defects from the chemical corrosion technology, specifically realize real-time observation and control in the chemical corrosion process, realize accurate positioning and observation of corrosion characteristics of various defects, and realize dynamic update and switching of corrosive liquid.
Disclosure of Invention
The invention aims to provide a device and a method for dynamically observing a tellurium-zinc-cadmium material chemical corrosion pit, simultaneously solve the defects of the existing chemical corrosion method in the aspects of process controllability, continuity, stability and the like, and provide an effective means for researching the structure and the generation mechanism of tellurium-zinc-cadmium defects and evaluating the defect revealing effects of different corrosive liquids.
The invention discloses a device and a method for dynamically observing a tellurium-zinc-cadmium material chemical corrosion pit. The method comprises the steps of fixing a sample in an optical observable corrosion tank, automatically injecting one or more corrosive liquids and cleaning liquids through an automatic liquid inlet unit, dynamically updating and sequentially switching, and immediately recovering waste liquid generated in the process by a waste liquid recovery unit, wherein the observation and measurement unit integrates a microscope, a CCD camera, measurement and control software and storage equipment, and performs real-time observation, collection, display and storage on microscopic processes of material corrosion.
The above object of the present invention is achieved by the following technical solutions:
the device for dynamically observing the tellurium-zinc-cadmium material chemical corrosion pit consists of a sample corrosion unit 1, an automatic liquid inlet unit 2, a waste liquid recovery unit 3 and an observation and measurement and control unit 4, and is characterized in that: the sample corrosion unit 1 consists of a corrosion tank 1-1, a main liquid inlet pipe 1-2, a corrosion liquid division liquid inlet pipe 1-3, a corrosion liquid inlet valve 1-4, a cleaning liquid division liquid inlet pipe 1-5, a cleaning liquid inlet valve 1-6, a liquid discharge pipe 1-7, a liquid discharge valve 1-8, a sealing ring 1-9, a tank cover 1-10 and a fixing screw, wherein the sample corrosion unit 1 is connected with an automatic liquid inlet unit 2 through the division liquid inlet pipes 1-3 and 1-5, and the sample corrosion unit 1 is connected with a waste liquid recovery unit 3 through the liquid discharge pipe 1-7; the automatic liquid inlet unit 2 consists of an etching liquid storage tank 2-1, an etching liquid inlet pump 2-2, a cleaning liquid storage tank 2-3 and a cleaning liquid inlet pump 2-4, wherein two ends of each liquid inlet pump are respectively connected with one liquid storage tank 2-1,2-3 and one liquid separating inlet pipe 1-3,1-5 through hoses, and the etching liquid and the cleaning liquid in the liquid storage tanks 2-1,2-3 can be automatically injected into the etching tank 1-1 simultaneously or sequentially by starting the automatic liquid inlet unit 2; the waste liquid recovery unit 3 consists of a waste liquid tank 3-1 and a liquid discharge pump 3-2, the liquid discharge pump 3-2 is respectively connected with the waste liquid tank 3-1 and a liquid discharge pipe 1-7 through hoses, and the liquid in the corrosion tank 1-1 can be automatically discharged into the waste liquid tank 3-1 by starting the waste liquid recovery unit 3; the observation and measurement and control unit 4 consists of a microscope, a CCD camera, measurement and control software and storage equipment, wherein the observation mode of the microscope can be switched between visible light reflection and infrared light transmission, the integral magnification is adjustable between 50 times and 1000 times, and the observation and measurement and control unit 4 can conduct real-time and dynamic observation and recording on the generation and evolution process of a material corrosion pit and the characteristics of material defects and corrosive liquid action.
Fixing a sample in a corrosion tank 1-1, covering a transparent tank cover 1-10, selecting a region to be corroded and observed by using a microscope, injecting a corrosive liquid into the corrosion tank 1-1 through a corrosive liquid inlet pump 2-2 to corrode the sample, starting a liquid discharge pump 3-2, continuously and alternately updating the corrosive liquid in the corrosion tank 1-1 in the corrosion process, simultaneously collecting the generated waste liquid in a waste liquid tank 3-1 in real time, dynamically observing and recording a material corrosion pit through the microscope and a CCD camera in the corrosion process to form an evolution state, and injecting a cleaning liquid into the corrosion tank 1-1 through a cleaning liquid inlet pump 2-4 after the corrosion is finished until the sample is cleaned.
The corrosion tank 1-1 is made of corrosion-resistant materials, and is in the shape of an irregular tank body with a certain depth, the right side of the tank body is connected with a main liquid inlet pipe 1-2, an inner hole of the main liquid inlet pipe is communicated with the inside of the corrosion tank 1-1, a plurality of corrosion liquid inlet pipes 1-3 and cleaning liquid inlet pipes 1-5 are separated by the main liquid inlet pipe 1-2, each liquid inlet pipe is provided with a liquid inlet valve which is independently controlled, the corrosion liquid inlet valves 1-4 and cleaning liquid inlet valves 1-6 are respectively used for controlling the inlet of various corrosion liquids and cleaning liquids, the lower part of the left side of the corrosion tank 1-1 is connected with a liquid discharge pipe 1-7, the inner hole of the liquid discharge pipe is communicated with the inside of the corrosion tank 1-1, and the liquid discharge pipe 1-7 is provided with a liquid discharge valve 1-8; threaded holes are formed in the periphery of the upper surface of the corrosion groove 1-1 and are used for installing fixing screws; the shape and the size of the upper surfaces of the groove cover 1-10 and the corrosion groove 1-1 are the same, the material is transparent, the optical observation can be realized, a plurality of through holes are formed in the periphery and correspond to the threaded holes on the upper surface of the corrosion groove 1-1, a corrosion-resistant sealing ring 1-9 is arranged between the corrosion groove 1-1 and the groove cover 1-10, a fixing screw is arranged, and the groove cover 1-10 and the corrosion groove 1-1 are sealed and fixed through the sealing ring 1-9; the corrosion groove 1-1 is a sealing groove body capable of microscopic observation, and the internal corrosive liquid and volatile gas thereof are not leaked, and meanwhile, a plurality of corrosive liquids and cleaning liquids are connected.
A method for dynamically observing a cadmium zinc telluride material chemical etch pit, comprising the steps of:
(1) Cutting the sample into proper sizes, and polishing to make the surface of the sample mirror-like bright;
(2) Cleaning the sample with boiled trichloroethylene for 3 times or more, cleaning the sample with methanol for 3 times or more, and drying with high-purity nitrogen;
(3) Preparing a bromomethanol solution with the bromine volume fraction of 5 per mill, putting a sample into the bromomethanol solution for corrosion for 15 seconds, then rapidly putting the sample into methanol for cleaning for 3 times or more, then cleaning the sample with deionized water for 3 times or more, and drying the sample with high-purity nitrogen;
(4) Placing the sample to be corroded surface upwards in the center of a corrosion groove 1-1, adhering and fixing the sample by using a corrosion-resistant adhesive tape, covering a groove cover 1-10, and fixing by using a fixing screw;
(5) Pouring the corrosive liquid required for preparation into a corrosive liquid storage tank 2-1, connecting with a corrosive liquid inlet pump 2-2, pouring the cleaning liquid required for preparation into a cleaning liquid storage tank 2-3, connecting with a cleaning liquid inlet pump 2-4, and connecting a waste liquid tank 3-1 with a liquid discharge pump 3-2;
(6) Turning on a microscope light source, placing a sample corrosion groove 1-1 on a microscope sample stage, selecting proper magnification, adjusting a focusing nut to focus the upper surface of a sample, observing the defect distribution condition of the sample, and selecting a region to be corroded and observed;
(7) The method comprises the steps that an etching liquid inlet pipe 1-3 and a cleaning liquid inlet pipe 1-5 of an etching tank are respectively connected with an etching liquid inlet pump 2-2 and a cleaning liquid inlet pump 2-4, a liquid discharge pipe 1-7 on the left side is connected with a liquid discharge pump 3-2, an etching liquid inlet valve 1-4 which is not connected with a liquid inlet unit is confirmed to be in a closed state, and a cleaning liquid inlet valve 1-6 and a liquid discharge valve 1-8 are confirmed to be in a closed state;
(8) Setting the flow rate of an etching liquid inlet pump 2-2, opening a corresponding liquid inlet valve 1-4, setting the flow rate of a liquid discharge pump 3-2, opening a liquid discharge valve 1-8, operating the etching liquid inlet pump 2-2 to start liquid injection, and operating the liquid discharge pump 3-2 to start liquid discharge after the etching liquid completely submerges the sample to be etched, wherein the sample is always in a submerged state in the etching process;
(9) The focal length of the microscope is properly fine-tuned, so that the microscope can clearly observe the surface of a sample all the time, the change process of a corrosion pit is displayed on a display through a CCD camera, and images and videos are acquired in real time to store data;
(10) After corrosion is finished, closing the corrosive liquid inlet pump 2-2 and the liquid inlet valve 1-4, setting the flow rate of the cleaning liquid inlet pump 2-4, opening the corresponding liquid inlet valve 1-6, adjusting the flow rate of the liquid discharge pump 3-2 to be matched, operating the cleaning liquid inlet pump 2-4 to start injecting cleaning liquid until the sample is cleaned, closing the cleaning liquid inlet pump 2-4 and the liquid inlet valve 1-6, and closing the liquid discharge pump 3-2 and the liquid discharge valve 1-8 when the liquid in the corrosive tank 1-1 is discharged completely;
(11) If a plurality of reagents are needed to be corroded or cleaned in sequence, repeating the steps (8) to (10);
(12) Classifying and recycling the residual chemical corrosive liquid, cleaning liquid and recycled chemical waste liquid, cleaning related experimental devices by using deionized water, and drying;
(13) The surface of the sample is dried by using high-purity nitrogen, and the appearance of corrosion pits on the surface of the sample is observed and statistically analyzed by using a microscope.
The invention has the following advantages:
(1) The dynamic visual observation can be realized, and the dynamic process from generation to disappearance of the corrosion pits of the recording material can be observed in real time;
(2) The method has strong functionality, can complete the multi-step corrosion cleaning process in situ under a fixed microscopic view field, and does not leave original chemical liquid in the corrosion tank when various corrosion liquids are switched;
(3) The stability is high, the dynamic update of the corrosive liquid in the corrosion process can be realized, and the corrosion state is kept stable;
(4) The process effect is good, and the corroded sample is not easy to oxidize.
Drawings
FIG. 1 is a flow chart of the apparatus of the present invention, wherein the sample is etched in the unit of FIG. 1; 1-1 etching a groove; 1-2 main liquid inlet pipe; 1-3, separating a corrosive liquid into liquid inlet pipes; 1-4 corrosive liquid inlet valve; 1-5 cleaning liquid separating and feeding pipe; 1-6 a cleaning liquid inlet valve; 1-7 liquid discharge pipes; 1-8 liquid discharge valves; 2 an automatic liquid inlet unit; 2-1 a corrosive liquid storage tank; 2-2, a corrosive liquid inlet pump; 2-3 a cleaning solution storage tank; 2-4 a cleaning solution feed pump; 3-a waste liquid recovery unit; 3-1 a waste liquid tank; 3-2 liquid discharge pump; and 4, observing the measurement and control unit.
FIG. 2 is a schematic diagram of a sample etching unit, in which 1-1 etching grooves are shown; 1-2 main liquid inlet pipe; 1-3, separating a corrosive liquid into liquid inlet pipes; 1-4 corrosive liquid inlet valve; 1-5 cleaning liquid separating and feeding pipe; 1-6 a cleaning liquid inlet valve; 1-7 liquid discharge pipes; 1-8 liquid discharge valves; 1-9 sealing rings; 1-10 groove covers.
Detailed Description
The invention is further illustrated by the following specific examples, which are provided to illustrate the invention and not to limit the scope of the invention in any way, and any modifications or variations that may be readily effected by one skilled in the art are intended to be included within the scope of the invention and the appended claims.
Example 1:
(1) The method comprises the steps of (211) cutting a tellurium-zinc-cadmium wafer processed along the surface (211) into 20mm X30 mm with the thickness of 1mm, firstly grinding the surface (211) B of a sample by using a 3-micrometer alumina aqueous solution to remove 50 mu m, and then performing chemical mechanical polishing by using Chemlox polishing solution to remove 20 mu m, so that the surface of the sample presents mirror-like brightness;
(2) Cleaning the sample 3 times by using boiled trichloroethylene, cleaning the sample 3 times by using methanol, and drying by using high-purity nitrogen;
(3) Preparing bromomethanol solution with the bromine volume fraction of 5 per mill, placing a sample (211) with the B surface facing upwards for corrosion for 15 seconds, then rapidly placing the sample into methanol for cleaning for 3 times, then cleaning the sample with deionized water for 3 times, and drying the sample with high-purity nitrogen;
(4) Placing the sample (211) with the B surface upwards in the center of the lower corrosion groove 1-1, adhering and fixing the sample by using a corrosion-resistant adhesive tape, covering the groove cover 1-10, and fixing by using a fixing screw;
(5) The preparation method comprises the following steps of: nitric acid: preparing Everson corrosive liquid according to the volume ratio of hydrofluoric acid of 100:20:5, uniformly stirring, pouring the prepared Everson corrosive liquid into a corrosive liquid storage tank 2-1, connecting with a corrosive liquid inlet pump 2-2, pouring deionized water into a cleaning liquid storage tank 2-3, connecting with a cleaning liquid inlet pump 2-4, and connecting a waste liquid tank 3-1 with a liquid discharge pump 3-2;
(6) Turning on a microscope light source, placing a sample corrosion groove 1-1 on a microscope sample stage, selecting a magnification factor of 100 times, adjusting a focusing nut to focus the upper surface of a sample, switching different microscope observation modes to observe the defect distribution condition of the sample, and selecting a region to be corroded and observed;
(7) The method comprises the steps that an etching liquid inlet pipe 1-3 of an etching tank and a cleaning liquid inlet pipe 1-5 of an etching liquid are respectively connected with an automatic liquid inlet unit, a liquid discharge pipe 1-7 on the left side is connected with a liquid discharge pump 3-2, an etching liquid inlet valve 1-4 which is not connected with the liquid inlet unit is confirmed to be in a closed state, and a cleaning liquid inlet valve 1-6 and a liquid discharge valve 1-8 are confirmed to be in a closed state;
(8) Setting the flow rate of a liquid inlet pump 2-2 for controlling Everson corrosive liquid to be 6ml/min, opening a corresponding liquid inlet valve 1-4, setting the flow rate of a liquid discharge pump 3-2 to be 6ml/min, opening a liquid discharge valve 1-8, operating the liquid inlet pump 2-2 to start liquid injection, operating the liquid discharge pump 3-2 to start liquid discharge after the corrosive liquid completely submerges a sample to be corroded, finely adjusting the flow rates of the liquid inlet pump 2-2 and the liquid discharge pump 3-2, maintaining the dynamic update of the chemical corrosive liquid in the corrosion tank 1-1, and enabling the sample to be always in a submerged state;
(9) In the corrosion process, the focal length of the microscope is properly finely adjusted, so that the microscope can clearly observe the surface of a sample all the time, the change process of a corrosion pit is displayed on a display through a CCD camera, and images and videos are acquired in real time to store data;
(10) After the corrosion time reaches 150 seconds, closing a liquid inlet pump 2-2 and a liquid inlet valve 1-4 for controlling Everson corrosion liquid, then opening the liquid inlet pump 2-4 and the liquid inlet valve 1-6 for controlling deionized water, setting the flow rate to be 30ml/min, adjusting the flow rate of a liquid discharge pump 3-2 to be 30ml/min, flushing a sample for 3min, closing a cleaning liquid inlet pump 2-4 and the liquid inlet valve 1-6, and closing the liquid discharge pump 3-2 and the liquid discharge valve 1-8 when liquid in the corrosion tank 1-1 is completely discharged;
(11) Classifying and recycling the residual chemical corrosive liquid, cleaning liquid and recycled chemical waste liquid, cleaning related experimental devices by using deionized water, and drying;
(12) The surface of the sample is dried by using high-purity nitrogen, and the appearance of corrosion pits on the surface of the sample is observed and statistically analyzed by using a microscope.
Example 2:
(1) The method comprises the steps of (1) cutting a tellurium-zinc-cadmium wafer processed along the (111) surface into 20mm X20 mm with the thickness of 3mm, firstly grinding the (111) A surface of a sample by using a 3-micrometer alumina aqueous solution to remove 30 mu m, and then performing chemical mechanical polishing by using Chemlox polishing solution to remove 15 mu m, so that the surface of the sample presents mirror-like brightness;
(2) Cleaning the sample 3 times by using boiled trichloroethylene, cleaning the sample 3 times by using methanol, and drying by using high-purity nitrogen;
(3) Preparing bromomethanol solution with the bromine volume fraction of 5 per mill, placing a sample (111) A face upwards, corroding for 15 seconds, then rapidly placing the sample into methanol for cleaning for 3 times, then cleaning for 3 times by deionized water, and drying by high-purity nitrogen;
(4) Placing the sample (111) A face upwards in the center of the lower corrosion groove 1-1, adhering and fixing the sample by using a corrosion-resistant adhesive tape, covering the groove cover 1-10, and fixing by using a fixing screw; the method comprises the steps of carrying out a first treatment on the surface of the
(5) Preparing Nakagawa corrosive liquid according to the volume ratio of water to hydrogen peroxide to hydrofluoric acid of 2:2:3, preparing E solution according to the volume ratio of nitric acid to water to potassium dichromate of 10ml to 4g, preparing EAg-1 corrosive liquid according to the volume ratio of E solution to silver nitrate of 10ml to 0.5mg, respectively pouring Nakagawa corrosive liquid and EAg-1 corrosive liquid into 2 corrosive liquid storage tanks 2-1, connecting with a corrosive liquid inlet pump 2-2, pouring deionized water into a cleaning liquid storage tank 2-3, connecting with a cleaning liquid inlet pump 2-4, and connecting a waste liquid tank 3-1 with a liquid discharge pump 3-2;
(6) Turning on a microscope light source, placing a sample corrosion groove 1-1 on a microscope sample stage, selecting an amplification factor of 200 times, adjusting a focusing nut to focus the upper surface of a sample, switching different microscope observation modes to observe the defect distribution condition of the sample, and selecting an area to be corroded and observed;
(7) The method comprises the steps that an etching liquid inlet pipe (1-3) of an etching tank and a cleaning liquid inlet pipe (1-5) of a cleaning liquid inlet pipe are respectively connected with an automatic liquid inlet unit, a liquid discharge pipe (1-7) on the left side is connected with a liquid discharge pump (3-2), an etching liquid inlet valve (1-4) which is not connected with the liquid inlet unit is confirmed to be in a closed state, and a cleaning liquid inlet valve (1-6) and a liquid discharge valve (1-8) are confirmed to be in a closed state;
(8) Setting the flow rate of a liquid inlet pump 2-2 for controlling Nakagawa corrosive liquid to be 4ml/min, opening a corresponding liquid inlet valve 1-4, setting the flow rate of a liquid discharge pump 3-2 to be 4ml/min, opening a liquid discharge valve 1-8, operating the liquid inlet pump 2-2 to start liquid injection, operating the liquid discharge pump 3-2 to start liquid discharge after the corrosive liquid completely submerges a sample to be corroded, finely adjusting the flow rates of the liquid inlet pump 2-2 and the liquid discharge pump 3-2, maintaining the dynamic update of the chemical corrosive liquid in the corrosion tank 1-1, and enabling the sample to be in a submerged state all the time;
(9) In the corrosion process, the focal length of the microscope is properly finely adjusted, so that the microscope can clearly observe the surface of a sample all the time, the change process of a corrosion pit is displayed on a display through a CCD camera, and images and videos are acquired in real time to store data;
(10) After the etching time reaches 45s, closing a liquid inlet pump 2-2 and a liquid inlet valve 1-4 for controlling Nakagawa etching liquid, then opening the liquid inlet pump 2-4 and the liquid inlet valve 1-6 for controlling deionized water, setting the flow rate to be 20ml/min, adjusting the flow rate of a liquid discharge pump 3-2 to be 20ml/min, flushing a sample for 2min, closing a cleaning liquid inlet pump 2-4 and the liquid inlet valve 1-6, and closing the liquid discharge pump 3-2 and the liquid discharge valve 1-8 when liquid in the etching tank 1-1 is discharged completely;
(11) Setting the flow rate of a liquid inlet pump 2-2 for controlling the corrosive liquid of the EAg-1 to be 5ml/min, opening a corresponding liquid inlet valve 1-4, setting the flow rate of a liquid discharge pump 3-2 to be 5ml/min, opening a liquid discharge valve 1-8, operating the liquid inlet pump 2-2 to start liquid injection, operating the liquid discharge pump 3-2 to start liquid discharge after the corrosive liquid completely submerges a sample to be corroded, finely adjusting the flow rates of the liquid inlet pump 2-2 and the liquid discharge pump 3-2, maintaining the dynamic update of the chemical corrosive liquid in the corrosion tank 1-1, and enabling the sample to be always in a submerged state;
(12) In the corrosion process, the focal length of the microscope is properly finely adjusted, so that the microscope can clearly observe the surface of a sample all the time, the change process of a corrosion pit is displayed on a display through a CCD camera, and images and videos are acquired in real time to store data;
(13) After the corrosion time reaches 30s, closing a liquid inlet pump 2-2 and a liquid inlet valve 1-4 for controlling EAg-1 corrosion liquid, then opening the liquid inlet pump 2-4 and the liquid inlet valve 1-6 for controlling deionized water, setting the flow rate to 25ml/min, adjusting the flow rate of a liquid discharge pump 3-2 to 25ml/min, flushing a sample for 3min, closing the liquid inlet pump 2-4 and the liquid inlet valve 1-6 for cleaning liquid, and closing the liquid discharge pump 3-2 and the liquid discharge valve 1-8 when the liquid in the corrosion tank 1-1 is completely discharged;
(14) Classifying and recycling the residual chemical corrosive liquid, cleaning liquid and recycled chemical waste liquid, cleaning related experimental devices by using deionized water, and drying;
(15) The surface of the sample is dried by using high-purity nitrogen, and the appearance of corrosion pits on the surface of the sample is observed and statistically analyzed by using a microscope.
Claims (2)
1. The device for dynamically observing the tellurium-zinc-cadmium material chemical corrosion pit consists of a sample corrosion unit (1), an automatic liquid inlet unit (2), a waste liquid recovery unit (3) and an observation and measurement and control unit (4), and is characterized in that:
the sample corrosion unit (1) consists of a corrosion groove (1-1), a main liquid inlet pipe (1-2), a corrosion liquid division liquid inlet pipe (1-3), a corrosion liquid inlet valve (1-4), a cleaning liquid division liquid inlet pipe (1-5), a cleaning liquid inlet valve (1-6), a liquid discharge pipe (1-7), a liquid discharge valve (1-8), a sealing ring (1-9), a groove cover (1-10) and a fixing screw, wherein the sample corrosion unit (1) is connected with an automatic liquid inlet unit (2) through the division liquid inlet pipe (1-3, 1-5), and the sample corrosion unit (1) is connected with a waste liquid recovery unit (3) through the liquid discharge pipe (1-7);
the automatic liquid inlet unit (2) consists of a plurality of corrosive liquid storage tanks (2-1), corrosive liquid inlet pumps (2-2), cleaning liquid storage tanks (2-3) and cleaning liquid inlet pumps (2-4), two ends of each liquid inlet pump are respectively connected with one liquid storage tank (2-1, 2-3) and one liquid separating inlet pipe (1-3, 1-5) through hoses, one or more corrosive liquids and cleaning liquids can be sequentially injected or simultaneously injected by starting the automatic liquid inlet unit (2), and the flow rate of the waste liquid recovery unit (3) is adjusted to dynamically update the corrosive liquids;
the waste liquid recovery unit (3) consists of a waste liquid tank (3-1) and a liquid discharge pump (3-2), the liquid discharge pump (3-2) is respectively connected with the waste liquid tank (3-1) and the liquid discharge pipe (1-7) through hoses, and the liquid in the corrosion tank (1-1) can be automatically discharged into the waste liquid tank (3-1) by starting the waste liquid recovery unit (3);
the observation and measurement and control unit (4) consists of a microscope, a CCD camera, measurement and control software and storage equipment, wherein the observation mode of the microscope is switched between visible light reflection and infrared light transmission, and the integral magnification is adjustable between 50 times and 1000 times;
placing a sample in a corrosion tank (1-1), selecting a region to be corroded and observed by using a microscope, injecting a corrosive liquid into the corrosion tank (1-1) through a corrosive liquid inlet pump (2-2), corroding the sample, starting a liquid discharge pump (3-2), continuously and alternately updating the corrosive liquid in the corrosion tank (1-1) in the corrosion process, simultaneously collecting the generated waste liquid in a waste liquid tank (3-1), dynamically observing and recording a material corrosion pit through the microscope and a CCD camera in the corrosion process to form an evolution state, and injecting a cleaning liquid into the corrosion tank (1-1) through a cleaning liquid inlet pump (2-4) after the corrosion is finished until the sample is cleaned;
the corrosion tank (1-1) is made of corrosion-resistant materials, the corrosion tank is in the shape of an irregular tank body with a certain depth, the right side of the tank body is connected with a main liquid inlet pipe (1-2), an inner hole of the main liquid inlet pipe is communicated with the inside of the corrosion tank (1-1), a plurality of corrosion liquid inlet pipes (1-3) and cleaning liquid inlet pipes (1-5) are separated from the main liquid inlet pipe (1-2), each liquid inlet pipe is provided with a liquid inlet valve which is independently controlled, each liquid inlet valve comprises a corrosion liquid inlet valve (1-4) and a cleaning liquid inlet valve (1-6), liquid inlets of various corrosion liquids and cleaning liquids are respectively controlled, the lower part of the left side of the corrosion tank (1-1) is connected with a liquid discharge pipe (1-7), the inner hole of the liquid discharge pipe is communicated with the inside of the corrosion tank (1-1), and the liquid discharge pipe (1-7) is provided with a liquid discharge valve (1-8); threaded holes are formed around the upper surface of the corrosion groove (1-1) and are used for installing fixing screws; the shape and the size of the upper surfaces of the groove cover (1-10) and the corrosion groove (1-1) are the same, the material is transparent, the groove cover can be used for optical observation, a plurality of through holes are formed in the periphery and correspond to threaded holes in the upper surface of the corrosion groove (1-1), a corrosion-resistant sealing ring (1-9) is arranged between the corrosion groove (1-1) and the groove cover (1-10), fixing screws are installed, and the groove cover (1-10) and the corrosion groove (1-1) are fixed in a sealing mode through the sealing ring (1-9); the corrosion groove (1-1) is a sealing groove body which can be observed microscopically, the internal corrosive liquid and volatile gas thereof have no leakage, and simultaneously, a plurality of corrosive liquids and cleaning liquids are connected.
2. A method for dynamically observing a cadmium zinc telluride material chemical etch pit based on an apparatus for dynamically observing a cadmium zinc telluride material chemical etch pit according to claim 1, comprising the steps of:
1) Cutting the sample into proper sizes, and polishing to make the surface of the sample mirror-like bright;
2) Cleaning the sample with boiled trichloroethylene for 3 times or more, cleaning the sample with methanol for 3 times or more, and drying with high-purity nitrogen;
3) Preparing a bromomethanol solution with the bromine volume fraction of 5 per mill, putting a sample into the bromomethanol solution for corrosion for 15 seconds, then rapidly putting the sample into methanol for cleaning for 3 times or more, then cleaning the sample with deionized water for 3 times or more, and drying the sample with high-purity nitrogen;
4) Placing a sample to be corroded surface upwards in the center of a corrosion groove (1-1), adhering and fixing the sample by using a corrosion-resistant adhesive tape, covering a groove cover (1-10), and fixing by using a fixing screw;
5) The method comprises the steps of preparing required corrosive liquid, pouring the corrosive liquid into a corrosive liquid storage tank (2-1), connecting with a corrosive liquid inlet pump (2-2), preparing required cleaning liquid, pouring the cleaning liquid into a cleaning liquid storage tank (2-3), connecting with a cleaning liquid inlet pump (2-4), and connecting a waste liquid tank (3-1) with a liquid discharge pump (3-2);
6) Turning on a microscope light source, placing a sample corrosion groove (1-1) on a microscope sample stage, selecting proper magnification, adjusting a focusing nut to focus the upper surface of a sample, respectively observing the inside and the surface of a material by using a microscope transmission mode and a microscope reflection mode, observing the defect distribution condition of the sample, and selecting a region to be corroded and observed;
7) The method comprises the steps that an etching liquid inlet pipe (1-3) and a cleaning liquid inlet pipe (1-5) of an etching tank are respectively connected with an etching liquid inlet pump (2-2) and a cleaning liquid inlet pump (2-4), a liquid discharge pipe (1-7) on the left side is connected with a liquid discharge pump (3-2), an etching liquid inlet valve (1-4) which is not connected with a liquid inlet unit is confirmed to be in a closed state, and a cleaning liquid inlet valve (1-6) and a liquid discharge valve (1-8) are confirmed to be in a closed state;
8) Setting the flow rate of an etching liquid inlet pump (2-2), opening a corresponding liquid inlet valve (1-4), setting the flow rate of a liquid discharge pump (3-2), opening a liquid discharge valve (1-8), operating the etching liquid inlet pump (2-2) to start liquid injection, operating the liquid discharge pump (3-2) to start liquid discharge after the etching liquid completely submerges a sample to be etched, and enabling the sample to be in a submerged state all the time in the etching process;
9) The focal length of the microscope is properly fine-tuned, the reflection mode and the transmission mode of the microscope are switched according to the requirement to dynamically observe the corrosion pit of the material to form an evolution state, so that the microscope can be always focused clearly, the change process of the corrosion pit is displayed on a display through a CCD camera, images and videos are collected in real time, and data are stored;
10 After corrosion is finished, closing the corrosive liquid inlet pump (2-2) and the liquid inlet valve (1-4), setting the flow rate of the cleaning liquid inlet pump (2-4), opening the corresponding liquid inlet valve (1-6), adjusting the flow rate of the liquid discharge pump (3-2) to be matched, operating the cleaning liquid inlet pump (2-4) to start to inject cleaning liquid until a sample is cleaned, closing the cleaning liquid inlet pump (2-4) and the liquid inlet valve (1-6), and closing the liquid discharge pump (3-2) and the liquid discharge valve (1-8) when the liquid in the corrosive tank (1-1) is discharged;
11 If multiple reagents are needed to be corroded or cleaned in sequence, repeating the steps 8) to 10);
12 Classifying and recycling the rest chemical corrosive liquid, cleaning liquid and the recycled chemical waste liquid, cleaning related experimental apparatuses by using deionized water, and drying;
13 Drying the surface of the sample by using high-purity nitrogen, and observing and statistically analyzing the corrosion pit morphology of the surface of the sample by using a microscope.
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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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