CN117779163A - Metallographic corrosion system for noble metals - Google Patents
Metallographic corrosion system for noble metals Download PDFInfo
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- CN117779163A CN117779163A CN202311829184.8A CN202311829184A CN117779163A CN 117779163 A CN117779163 A CN 117779163A CN 202311829184 A CN202311829184 A CN 202311829184A CN 117779163 A CN117779163 A CN 117779163A
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- flue gas
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- waste flue
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- 230000007797 corrosion Effects 0.000 title claims abstract description 227
- 238000005260 corrosion Methods 0.000 title claims abstract description 227
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 40
- 239000002699 waste material Substances 0.000 claims abstract description 58
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000003546 flue gas Substances 0.000 claims abstract description 54
- 238000011084 recovery Methods 0.000 claims abstract description 43
- 238000001914 filtration Methods 0.000 claims abstract description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000011521 glass Substances 0.000 claims description 93
- 238000007789 sealing Methods 0.000 claims description 27
- 238000010521 absorption reaction Methods 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000000605 extraction Methods 0.000 claims description 15
- 238000005530 etching Methods 0.000 claims description 11
- 230000000149 penetrating effect Effects 0.000 claims description 11
- 239000000779 smoke Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 5
- 239000007770 graphite material Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims 1
- 238000013461 design Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 12
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 8
- 229910052801 chlorine Inorganic materials 0.000 description 8
- 230000001105 regulatory effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 229920001971 elastomer Polymers 0.000 description 5
- 238000003780 insertion Methods 0.000 description 5
- 230000037431 insertion Effects 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000003595 mist Substances 0.000 description 4
- 238000004804 winding Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
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Abstract
The invention discloses a metallographic corrosion system, in particular discloses a metallographic corrosion system for noble metals, and belongs to the technical field of design and manufacture of noble metal processing equipment. The metallographic corrosion system for the noble metal is safe in corrosion operation, has very limited influence on the surrounding environment and can effectively improve the corrosion efficiency. The metallographic corrosion system comprises a sealed corrosion device and a waste flue gas recovery and filtration device, wherein an electrolytic corrosion solution is arranged in the sealed corrosion device, waste flue gas generated by dissolving and corroding noble metals through electrolytic corrosion in the sealed corrosion device is recovered and filtered under the cooperation of the waste flue gas recovery and filtration device and then is discharged, and the electrolytic corrosion solution consists of 75% by volume of AR grade concentrated hydrochloric acid and 25% by volume of saturated sodium chloride solution.
Description
Technical Field
The invention relates to a metallographic corrosion system, in particular to a metallographic corrosion system for noble metals, and belongs to the technical field of design and manufacture of noble metal processing equipment.
Background
In the metallographic corrosion process of noble metals, a constant temperature Wang Shuiyu or hydrochloric acid electrolysis method is generally adopted for the corrosion of noble metal samples. There are certain limitations: constant temperature Wang Shuiyu can splash and volatilize a large amount of acid mist at the in-process of heating, along with the progress of corrosion process, aqua regia concentration reduces, and the corrosion effect descends, is difficult to carry out the technology solidification of corrosion time, and the aqua regia that splashes has certain hidden danger to operating personnel's health and safety, also is inconvenient to observe at the in-process of corrosion. The hydrochloric acid electrolysis needs to electrify the sample, for large-size samples, the sample to be corroded can be cured in advance through the curing agent, one end of the sample leaks out of the curing agent, and the leaked part is connected with the electrode to carry out electrolytic corrosion; however, for samples with small thickness direction sizes, such as thin sheet plates and failure samples on thin pipe walls, which need to be observed in a plane, due to the small thickness, the curing agent cannot leak, and electrolytic corrosion cannot be performed in this way, due to the limitations of electrolytic corrosion, volatilization of hydrochloric acid and chlorine exists in the process of performing, after the concentration of the hydrochloric acid is reduced, the corrosion effect is reduced, and certain hidden hazards exist for health and safety of operators.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the metallographic corrosion system for the noble metal is safe in corrosion operation, has very limited influence on the surrounding environment and can effectively improve the corrosion efficiency.
The technical scheme adopted for solving the technical problems is as follows: a metallographic corrosion system for noble metal comprises a sealed corrosion device and a waste flue gas recovery and filtration device, wherein electrolytic corrosion solution is arranged in the sealed corrosion device, noble metal is corroded by the electrolytic corrosion solution in the sealed corrosion device, the generated waste flue gas is recovered, filtered and discharged under the cooperation of the waste flue gas recovery and filtration device,
wherein the electrolytic corrosion solution consists of an AR grade concentrated hydrochloric acid with a volume fraction of 75% and a saturated sodium chloride solution with a volume fraction of 25%.
Further, the waste flue gas recovery and filtration device carries out recovery and filtration treatment on waste flue gas through an absorption liquid arranged in the waste flue gas recovery and filtration device, wherein the absorption liquid consists of a sodium hydroxide solution with the concentration of 100 mg/L.
The sealed corrosion device also comprises an electrode assembly, an corrosion product arrangement rack and a closable corrosion container assembly, wherein electrolytic corrosion solution is arranged in the corrosion container assembly, noble metals to be corroded are arranged in the corrosion container assembly through the corrosion product arrangement rack, the electrode assembly is inserted into the corrosion container assembly from the top, and a gas input end of the waste flue gas recovery filtering device is connected with the corrosion container assembly.
Further, the electrode assembly comprises a positive electrode rod and a negative electrode rod which are made of graphite materials, an insulating operation head is screwed on one end of the positive electrode rod which is not inserted into the corrosion container assembly, and a holding-back groove is formed in the insulating operation head.
The preferable mode of above-mentioned scheme is, the corrosion container subassembly includes corrosion glass container and corrosion glass lid, be provided with corrosion article arrangement frame and pass hole and useless flue gas and take out the connecting hole on corrosion glass container's lateral wall, be provided with electrode assembly patchhole on corrosion glass lid, corrosion glass container open top is sealed through corrosion glass lid, the corrosion article arrangement frame that the both ends were worn out corrosion glass container passes hole activity arrangement through corrosion article arrangement frame on corrosion glass container, positive pole stick and negative pole stick are respectively through electrode assembly patchhole detachable arrangement in corrosion glass container, useless flue gas recovery filter equipment's flue gas output is connected with useless flue gas and takes out the connecting hole.
Further, the open top of the corrosion glass container is of a circular structure with internal threads, a threaded boss which is matched with the circular structure is arranged on the corrosion glass cover, and the corrosion glass cover is screwed on the circular structure through the threaded boss; sealing members are arranged on the positive electrode rod and the negative electrode rod, and the gap between the positive electrode rod and the electrode assembly inserting hole and the gap between the negative electrode rod and the electrode assembly inserting hole are sealed by the sealing members.
The corrosion product arrangement frame comprises a corrosion fixing groove, a connecting support rod group, a closed adjusting plate group and a supporting operation rod group, wherein the corrosion fixing groove is arranged on the closed adjusting plate group through the connecting support rod groups which are arranged at two sides of the corrosion fixing groove along the radial direction; the etched article arrangement frame passes through the hole to be sealed under the cooperation of the sealing adjusting plate group,
the supporting operation rod group comprises a push-pull operation handle and a supporting auxiliary rod, the connecting support rod group comprises two connecting support rods, the sealing adjusting plate group comprises two sealing adjusting plates, the supporting auxiliary rod is L-shaped, the push-pull operation handle is connected with the sealing adjusting plate on one side through one end without the operation handle, the L-shaped supporting auxiliary rod is connected with the sealing adjusting plate on the other side through the free end on the long side, the two sealing adjusting plates are respectively connected with the two sides of the corrosion fixing groove along the radial direction through one connecting support rod,
one of the corrosion product arrangement frames outside the corrosion glass container passes through the hole to be provided with a sealing limit clamping plate.
Further, the waste flue gas recovery and filtration device comprises a waste flue gas recovery and filtration structure and a connecting pipe connected with a ball valve in series, wherein the waste flue gas recovery and filtration structure is connected with a waste flue gas extraction connecting hole through the connecting pipe, and the absorption liquid is arranged in the waste flue gas recovery and filtration structure.
The preferred mode of above-mentioned scheme is, and waste flue gas retrieves filtration includes filter glass container, filter glass lid and manometer, and the connecting pipe is connected with filter glass container from the side, and the filter glass lid that the open top of filter glass container passed through seals, and the pressure value in the filter glass container is measured through the manometer of arranging on the filter glass lid.
Further, an exhaust port and an air extraction interface are also arranged on the pressure gauge measurement, and a vacuum pump is connected to the air extraction interface.
The beneficial effects of the invention are as follows: the technical scheme that this application provided is through setting up one set including sealed corrosion device and waste flue gas recovery filter equipment's metallographic corrosion system, then arrange electrolytic corrosion solution in this sealed corrosion device again to corrode noble metal through electrolytic corrosion solution in sealed corrosion device, the waste flue gas that produces is retrieved under waste flue gas recovery filter equipment's cooperation and is filtered the back and discharge, and wherein electrolytic corrosion solution comprises 75% volume fraction's AR level concentrated hydrochloric acid +25% volume fraction's saturated sodium chloride solution. That is, the present application is based on the electrolytic corrosion principle, improves the existing common electrolytic corrosion, makes the electrolytic corrosion proceed in a sealable corrosion device, and on this basis, recovers and filters the waste flue gas generated by corrosion through a waste flue gas recovery filter device, and then discharges.
Drawings
FIG. 1 is a schematic three-dimensional structure of a metallographic etching system for noble metals according to the present invention;
FIG. 2 is a schematic view of the three-dimensional structure of the other side of the metallographic etching system for noble metals according to the present invention;
FIG. 3 is a schematic view of the three-dimensional structure of the corrosion vessel assembly and the combination with the electrode assembly involved in the metallographic corrosion system for noble metals of the present invention;
FIGS. 4 and 5 are schematic diagrams of three-dimensional structures of two states of a corrosion glass container and a corrosion product arrangement frame combination, which are related to a metallographic corrosion system for noble metals;
FIG. 6 is a schematic three-dimensional view of the etched article placement frame involved in the metallographic etching system for noble metals according to the present invention;
FIG. 7 is a schematic view of the three-dimensional structure of an electrode assembly involved in the metallographic etching system for noble metals of the present invention;
FIG. 8 is a schematic three-dimensional structure of a waste flue gas recovery filter device involved in the metallographic corrosion system for noble metals of the present invention.
Marked in the figure as: the cathode rod 1, the anode rod 2, the insulating operation head 3, the holding groove 4, the corroded glass container 5, the corroded glass cover 6, the corroded arrangement frame penetrating hole 7, the waste smoke extraction connecting hole 8, the electrode assembly inserting hole 9, the corroded fixing groove 10, the push-pull operation handle 11, the supporting auxiliary rod 12, the connecting supporting rod 13, the sealing adjusting plate 14, the sealing limiting clamping plate 15, the ball valve 16, the connecting pipe 17, the filtered glass container 18, the filtered glass cover 19, the pressure gauge 20, the exhaust port 21 and the air extraction interface 22.
Detailed Description
As shown in figures 1-8, the metallographic corrosion system for noble metals provided by the invention is safe in corrosion operation, has very limited influence on the surrounding environment and can effectively improve the corrosion efficiency. The metallographic corrosion system comprises a sealed corrosion device and a waste flue gas recovery and filtration device, wherein an electrolytic corrosion solution is arranged in the sealed corrosion device, noble metals are corroded in the sealed corrosion device through the electrolytic corrosion solution, and generated waste flue gas is recovered and filtered under the cooperation of the waste flue gas recovery and filtration device and then is discharged, wherein the electrolytic corrosion solution consists of 75% by volume of AR grade concentrated hydrochloric acid and 25% by volume of saturated sodium chloride solution. That is, the present application is based on the electrolytic corrosion principle, improves the existing common electrolytic corrosion, makes the electrolytic corrosion proceed in a sealable corrosion device, and on this basis, recovers and filters the waste flue gas generated by the corrosion by a waste flue gas recovery filter device, and then discharges. Correspondingly, in order to improve the recovery effect of waste flue gas, the waste flue gas recovery filtering device of the application carries out recovery filtering treatment on waste flue gas through the absorption liquid arranged in the waste flue gas recovery filtering device, wherein the absorption liquid consists of sodium hydroxide solution with the concentration of 100 mg/L.
Further, in combination with the noble metal to be corroded by the present application, the noble metal is of a small decorative structure compared with the structure of articles used in production and living, and meanwhile, for convenient manufacture and subsequent use, the sealed corrosion device further comprises an electrode assembly, an corroding article arrangement frame and a closable corrosion container assembly, an electrolytic corrosion solution is arranged in the corrosion container assembly, the noble metal to be corroded is arranged in the corrosion container assembly through the corroding article arrangement frame, a negative electrode of the electrode assembly is inserted into the corrosion container assembly from the top, a positive electrode is in contact with an corroding article in the corroding article arrangement frame, and a gas input end of the waste flue gas recovery filtering device is connected with the corrosion container assembly. More specifically, the electrode assembly comprises a positive electrode rod 2 and a negative electrode rod 1 which are made of graphite materials, an insulating operation head 3 is screwed on one end of the positive electrode rod 2 which is not inserted into the corrosion container assembly, and a holding groove 4 is arranged on the insulating operation head 3. The corrosion container assembly comprises a corrosion glass container 5 and a corrosion glass cover 6, corrosion product arrangement frames penetrating through holes 7 and waste smoke extraction connecting holes 8 are formed in the side wall of the corrosion glass container 5, electrode assembly insertion holes 9 are formed in the corrosion glass cover 6, the open top of the corrosion glass container 5 is closed through the corrosion glass cover 6, corrosion product arrangement frames penetrating out of the corrosion glass container 5 at two ends are movably arranged on the corrosion glass container 5 through the corrosion product arrangement frames penetrating through the holes 7, an anode rod 2 and a cathode rod 1 are detachably arranged in the corrosion glass container 5 through the electrode assembly insertion holes 9 respectively, and the smoke output end of the waste smoke recovery filtering device is connected with the waste smoke extraction connecting holes 8 through connecting pipes 17. The corrosion product arrangement frame comprises a corrosion fixing groove 10, a connecting support rod group, a closed adjusting plate group and a supporting operation rod group, wherein the corrosion fixing groove 10 is arranged on the closed adjusting plate group through the connecting support rod groups which are arranged at two sides of the corrosion fixing groove in the radial direction, the supporting operation rod group is arranged at two ends of the closed adjusting plate group and is vertically coplanar with the connecting support rod group along the horizontal direction, and the corrosion fixing groove 10 in the corrosion glass container 5 is supported on the corrosion product arrangement frame penetrating hole 7 through the supporting operation rod group of which the two ends penetrate through the corrosion product arrangement frame penetrating hole 7; the corrosion product arrangement frame passes through the hole 7 to be sealed under the cooperation of sealing the regulating plate group, the support operating lever group includes a push-pull operating handle 11 and a support auxiliary rod 12, the connecting rod group includes two connecting rods 13, the sealing regulating plate group includes two sealing regulating plates 14, the support auxiliary rod 12 is L type, the push-pull operating handle 11 is connected with the sealing regulating plate 14 of one side through the one end that does not set up the operating handle, the free end of L type support auxiliary rod 12 passes through the free end of long limit is connected with the sealing regulating plate 14 of opposite side, two sealing regulating plates 14 are connected with the both sides of corrosion fixed slot 10 along radial direction through a connecting rod 13 respectively, be provided with sealed spacing cardboard 15 in one of them corrosion product arrangement frame that corrodes the glass container 5 outside passes through hole 7 department. The more preferable structure is that the open top of the corrosion glass container 5 is a circular structure with internal threads, a threaded boss which is suitable for the circular structure is arranged on the corrosion glass cover 6, and the corrosion glass cover 6 is screwed on the circular structure through the threaded boss; seals are provided on both the positive electrode rod 2 and the negative electrode rod 1, and both the gap between the positive electrode rod 2 and the electrode assembly insertion hole 9 and the gap between the negative electrode rod 1 and the electrode assembly insertion hole 9 are closed by the seals.
As another important improvement part of the present application, the waste flue gas recovery filter device includes a waste flue gas recovery filter structure and a connecting pipe 17 connected in series with a ball valve 16, the waste flue gas recovery filter structure is connected with the waste flue gas extraction connecting hole 8 through the connecting pipe 17, and the absorption liquid is arranged in the waste flue gas recovery filter structure. At this time, the waste gas recovery filter structure preferably includes a filter glass container 18, a filter glass cover 19, and a pressure gauge 20, the connection pipe 17 is connected to the filter glass container 18 from the side, the open top of the filter glass container 18 is closed by the filter glass cover 19, and the pressure value in the filter glass container 18 is measured by the pressure gauge 20 disposed on the filter glass cover 19. In order to facilitate the discharge of qualified gas, the pressure gauge 20 is further provided with a discharge port 21 and an air extraction interface 22, and the air extraction interface 22 is connected with a vacuum pump.
To sum up, the above-mentioned technical scheme that this application provided can realize noble metal sample corruption of different materials such as small-size thin slice, reduces the time of inlaying, slows down the speed that hydrochloric acid concentration becomes low, prevents that harmful gas from inhaling the human body, obtains better corrosion effect, promotes corrosion efficiency widely, and the mould is changed simply, easy and simple to handle.
The technical scheme of the application is further described by the following specific examples:
through the design, the corrosive liquid is placed in a transparent glass vessel, namely the corrosive glass vessel, the side surface of the glass vessel is provided with a drawing type plugboard for placing a sample to be corroded, namely the corrosion product arrangement frame, and the drawing type plugboard can move in the vertical and horizontal directions to realize the processes of lofting and sampling. The upper part of the glassware is covered by a screwed and unscrewed glass cover, a negative electrode material and a positive electrode material are inserted on the glass cover, so that the electrifying in the corrosion process is realized, and most of chlorine gas and volatilized acid mist generated in the corrosion process are left in the glassware through the design of the plugboard and the glass cover; and the diluted sodium hydroxide solution with certain concentration is placed in another transparent glass vessel II, namely the filter glass container, the upper part of the glass vessel is covered by a glass cover with a gasket, the upper part of the glass cover is connected with small-sized vacuumizing equipment, the glass vessel I and the glass vessel II are connected by a ball valve and a pipeline, the glass vessel II is pre-vacuumized before corrosion, the valve is closed, the glass vessel II is under negative pressure, after the glass vessel I is corroded, the valve is opened, waste gas enters the glass vessel II through the pipeline and is absorbed by the sodium hydroxide solution, so that the emission of chlorine and acid mist is reduced, the safety and health hidden danger of operators are reduced, the corrosion aim of samples with different sizes can be realized, the metallographic preparation problem of sheet samples is effectively solved, and the overall electrolytic corrosion efficiency is obviously improved. The metallographic corrosion system can realize good metallographic corrosion effect of a sheet sample, can realize recovery treatment of acid mist and chlorine generated in the corrosion process, and is simple and convenient to operate, and materials and solutions can be replaced quickly.
The glass corrosion container shell, namely glass ware, is shown in figure 3, the external dimension is 100 multiplied by 100mm, an internal thread is arranged at the top, a glass cover can be screwed, an external thread and the internal thread are arranged at the bottom to be matched with each other in a screwing and unscrewing way, two through holes are formed above the screwed glass cover, the diameter of the through hole matched with a negative electrode is 10.2mm, the diameter of the part of the negative electrode, inserted into a top cover, is 10mm, a rubber gasket and a negative electrode lead winding part are sleeved on the negative electrode, the inner diameter of the rubber gasket is 10mm, the outer diameter of the rubber gasket is 15mm, and the through hole is sealed by the self weight of the material of the negative electrode; the diameter of the through hole matched with the positive electrode is 10mm, the diameter of the insertion part of the positive electrode is 5mm, a winding part of the positive electrode wire is arranged on the positive electrode, a rubber gasket with the inner diameter of 5mm and the outer diameter of 10mm is sleeved on the positive electrode, so that the through hole is in sealing in the vertical movement process of the positive electrode, the whole positive electrode is made of graphite, the bottom of insulating plastic at the top of the positive electrode is provided with external threads, the insulating plastic can be matched with the internal threads at the top of the positive electrode, a pair of grooves are formed in the insulating plastic, the operation is convenient, a pair of square through holes are formed in the side wall of a glass corrosion container shell, the size is 6 multiplied by 20mm, the groove is used for the movement of a plugboard, and a pipeline with external threads is 20mm in outer diameter and is connected with a flange.
The whole structure of the glass plugboard is shown in fig. 6, the structure of the glass plugboard matched with the corrosion container hole is shown in fig. 4 and 5, wherein finger contact points are arranged at one end of the push-pull plugboard, the first baffle plate, the second baffle plate and the third baffle plate on the supporting auxiliary rod are cuboid with the length of 22mm and the width of 10mm, the size of the cuboid is slightly larger than that of the hole, the horizontal movement of the plugboard can be limited, the bottom of the corrosion fixing groove adopts a hollow ring, a surface to be corroded of a sample can be contacted with corrosive liquid, the width of the ring is 2mm, various designs can be carried out on the corrosion fixing groove according to the shape and the size of a commonly used sample, a contact with the diameter of 7mm is arranged at the bottom of a negative electrode, the inner diameter of the hollow ring is 8mm, the hollow ring of the corrosion fixing groove and the contact at the bottom of a positive electrode can be concentric by adjusting the position of the plugboard, and the contact can be inserted into the corrosion fixing groove.
The matching state of the plugboard and the corrosion container is shown in figure 5, in this state, the contact can be inserted into the corrosion fixing groove, the first sealing adjusting plate is clung to the inner wall of the corrosion container, the second sealing adjusting plate is clung to the outer wall of the corrosion container, and the sealing of the hole is realized. Because the first hole and the second hole are limited by the sizes of the second closed regulating plate and the first closed regulating plate, the plugboard cannot move to the left again, so that the hollow circular ring and the contact are positioned conveniently. This state is the state when the etching proceeds. When the insert plate and the corrosion container were in the first mating state and the sample was placed in the corrosion fixing groove, a surface 1mm higher than the bottom surface of the sample was defined as a standard liquid surface.
The second matching state of the plugboard and the corrosion container is shown in fig. 4, the corrosion fixing groove is arranged outside the corrosion container in the second matching state, a sample can be placed, the sealing adjusting plate III is arranged outside the corrosion container, and due to the size limitation of the hole, the sealing adjusting plate III can not move to the right again after contacting with the outer wall of the corrosion container, so that the plugboard can be prevented from shaking in the hollow round bad lofting process, and the lofting efficiency is improved.
The whole structure of the absorption container is shown in fig. 8, wherein the base of the absorption container mainly contains absorption liquid, the rubber gasket is placed between the top cover of the absorption container and the base of the absorption container, the top cover and the base are made of glass, semicircular annular grooves are formed in the contact surface between the lower part of the top cover and the gasket, semicircular annular grooves are formed in the contact surface between the upper part of the base and the gasket, the gasket is convenient to fix, the lower part of the pressure gauge is connected and fixed with the absorption container, two external pipelines are respectively arranged on two sides of the pressure gauge, one interface of the pressure gauge is connected with a vacuum pump, a valve is arranged at the other interface, the side of the pressure gauge is identical to the atmosphere, and a pipeline with external threads is arranged on the side wall of the base of the absorption container so as to be connected with a flange.
The whole view of the device is shown in fig. 1 and 2, two ends of the ball valve are respectively connected with the glass corrosion container through two sections of connecting pipelines under the cooperation of two flanges, and the outer walls of the two ends of the pipelines are provided with threads, so that the ball valve is conveniently connected through the threads.
Example 1
a) And (3) lofting: pressing the contact point of the plugboard, drawing the plugboard out to enable the plugboard to be in a second matching state, placing the polished sample in a hollow round defect of the corrosion fixing groove, pressing the contact point again, feeding the plugboard into the corrosion fixing groove, enabling the plugboard to be in the first matching state, winding and fixing the positive electrode wire below the middle upper part insulating plastic of the positive electrode, and winding and fixing the negative electrode wire to the middle upper part of the negative electrode.
b) Preparing a corrosive liquid: the corrosion container consists of an AR grade concentrated hydrochloric acid solution with the volume fraction of 75 percent and a saturated sodium chloride solution with the volume fraction of 25 percent, a top cover of the corrosion container is opened, and the corrosion liquid is continuously added until the standard liquid level is reached; preparing an absorption liquid: consists of 100mg/L sodium hydroxide solution, the top cover of the absorption tank is opened, and the absorption liquid is continuously added to a position which is 5mm lower than the lower edge of the pipeline. After the corrosive liquid and the absorption liquid are added, the top cover is opened respectively.
c) Closing the ball valve, opening a vacuum pump connected to the pressure gauge, closing a valve connected to the other interface of the pressure gauge, pumping out part of air in the absorption container, and closing the vacuum pump after the air pressure gauge number is slightly lower than the atmospheric pressure, wherein the inside of the absorption tank is in a negative pressure state.
d, 25V direct current is introduced, the insulating plastic on the positive electrode is pressed, the positive electrode is controlled to descend until the contact is contacted with the sample, corrosion starts in the contact process, chlorine is generated, most of the chlorine is left in the corrosion container because the corrosion container is in a sealed state, the concentration of the corrosion liquid is also reduced more slowly, and the use frequency of the corrosion liquid is prolonged. And after the corrosion time reaches 40s, controlling the anode to rise so as to separate the contact from the surface of the sample, and ending the corrosion.
e) And the spherical valve is opened, and most of chlorine is pumped into the absorption container because the inside of the absorption container is in a negative pressure state, and the chlorine reacts with sodium hydroxide to absorb most of the chlorine. After the reaction is fully carried out, a valve at the other interface of the pressure gauge is opened, and after the observed pressure representation number is restored to the standard atmospheric pressure, the valve at the other interface of the pressure gauge is closed.
f) C-e, sequentially corroding other samples, taking out the samples after the experiment is finished, performing metallographic observation, and discharging the waste liquid to a designated safe position.
Claims (10)
1. A metallographic etching system for noble metal, its characterized in that: the metallographic corrosion system comprises a sealed corrosion device and a waste flue gas recovery and filtration device, wherein electrolytic corrosion solution is arranged in the sealed corrosion device, waste flue gas generated by corroding noble metal in the sealed corrosion device through the electrolytic corrosion solution is recovered and filtered under the cooperation of the waste flue gas recovery and filtration device and then is discharged,
wherein the electrolytic corrosion solution consists of an AR grade concentrated hydrochloric acid with a volume fraction of 75% and a saturated sodium chloride solution with a volume fraction of 25%.
2. The metallographic corrosion system for noble metals according to claim 1, wherein: the waste flue gas recovery and filtration device carries out recovery and filtration treatment on waste flue gas through an absorption liquid arranged in the waste flue gas recovery and filtration device, wherein the absorption liquid consists of a sodium hydroxide solution with the concentration of 100 mg/L.
3. Metallographic corrosion system for noble metals according to claim 1 or 2, characterised in that: the sealed corrosion device also comprises an electrode assembly, an etching product arrangement rack and a closable corrosion container assembly, wherein the electrolytic corrosion solution is arranged in the corrosion container assembly, noble metals to be corroded are arranged in the corrosion container assembly through the etching product arrangement rack, the electrode assembly is inserted into the corrosion container assembly from the top, and the gas input end of the waste flue gas recovery filtering device is connected with the corrosion container assembly.
4. A metallographic etching system for noble metals according to claim 3, wherein: the electrode assembly comprises a positive electrode rod (2) and a negative electrode rod (1) which are made of graphite materials, an insulating operation head (3) is screwed on one end of the positive electrode rod (2) which is not inserted into the corrosion container assembly, and a holding groove (4) is formed in the insulating operation head (3).
5. The metallographic etching system for noble metals according to claim 4, wherein: the corrosion container assembly comprises a corrosion glass container (5) and a corrosion glass cover (6), corrosion product arrangement frames penetrating through holes (7) and waste smoke extraction connecting holes (8) are formed in the side wall of the corrosion glass container (5), electrode assembly inserting holes (9) are formed in the corrosion glass cover (6), the open top of the corrosion glass container (5) is sealed through the corrosion glass cover (6), corrosion product arrangement frames penetrating out of the corrosion glass container (5) at two ends are movably arranged on the corrosion glass container (5) through the corrosion product arrangement frames penetrating through the holes (7), the positive electrode rods (2) and the negative electrode rods (1) are detachably arranged in the corrosion glass container (5) through the electrode assembly inserting holes (9) respectively, and the smoke input end of the waste smoke recovery filtering device is connected with the waste smoke extraction connecting holes (8).
6. The metallographic etching system for noble metals according to claim 5, wherein: the open top of the corrosion glass container (5) is of a circular structure with internal threads, a threaded boss which is matched with the circular structure is arranged on the corrosion glass cover (6), and the corrosion glass cover (6) is screwed on the circular structure through the threaded boss; sealing elements are arranged on the positive electrode rod (2) and the negative electrode rod (1), and the gap between the positive electrode rod (2) and the electrode assembly inserting hole (9) and the gap between the negative electrode rod (1) and the electrode assembly inserting hole (9) are sealed through the sealing elements.
7. The metallographic corrosion system for noble metals according to claim 6, wherein: the corrosion product arrangement frame comprises a corrosion fixing groove (10), a connecting support rod group, a closed adjusting plate group and a supporting operation rod group, wherein the corrosion fixing groove (10) is arranged on the closed adjusting plate group through the connecting support rod groups which are arranged at two sides of the corrosion fixing groove in the radial direction, the supporting operation rod group is arranged at two ends of the closed adjusting plate group and is vertically coplanar with the connecting support rod group along the horizontal direction, and the corrosion fixing groove (10) positioned in the corrosion glass container (5) is supported on the corrosion product arrangement frame penetrating hole (7) through the supporting operation rod group of which the two ends penetrate out of the corrosion product arrangement frame penetrating hole (7); the etched article arrangement frame passes through the hole (7) to be sealed under the cooperation of the sealing adjusting plate group,
the supporting operation rod group comprises a push-pull operation handle (11) and a supporting auxiliary rod (12), the connecting support rod group comprises two connecting support rods (13), the closed adjusting plate group comprises two closed adjusting plates (14), the supporting auxiliary rod (12) is L-shaped, the push-pull operation handle (11) is connected with the closed adjusting plates (14) on one side through one end without the operation handle, the L-shaped supporting auxiliary rod (12) is connected with the closed adjusting plates (14) on the other side through the free end on the long side, the two closed adjusting plates (14) are respectively connected with the two sides of the corrosion fixing groove (10) along the radial direction through one connecting support rod (13),
one of the corrosion product arrangement frames outside the corrosion glass container (5) passes through the hole (7) to be provided with a sealing limit clamping plate (15).
8. The metallographic corrosion system for noble metals according to claim 7, wherein: the waste flue gas recovery and filtration device comprises a waste flue gas recovery and filtration structure and a connecting pipe (17) connected with a ball valve (16) in series, wherein the waste flue gas recovery and filtration structure is connected with a waste flue gas extraction connecting hole (8) through the connecting pipe (17), and absorption liquid is arranged in the waste flue gas recovery and filtration structure.
9. The metallographic corrosion system for noble metals according to claim 8, wherein: the waste flue gas recycling and filtering structure comprises a filter glass container (18), a filter glass cover (19) and a pressure gauge (20), wherein the connecting pipe (17) is connected with the filter glass container (18) from the side face, the open top of the filter glass container (18) is closed by the filter glass cover (19), and the pressure value in the filter glass container (18) is measured by the pressure gauge (20) arranged on the filter glass cover (19).
10. The metallographic corrosion system for noble metals according to claim 9, wherein: the pressure gauge (20) is also provided with a discharge port (21) and an air extraction interface (22), and the air extraction interface (22) is connected with a vacuum pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311829184.8A CN117779163A (en) | 2023-12-27 | 2023-12-27 | Metallographic corrosion system for noble metals |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311829184.8A CN117779163A (en) | 2023-12-27 | 2023-12-27 | Metallographic corrosion system for noble metals |
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| Publication Number | Publication Date |
|---|---|
| CN117779163A true CN117779163A (en) | 2024-03-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311829184.8A Pending CN117779163A (en) | 2023-12-27 | 2023-12-27 | Metallographic corrosion system for noble metals |
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| Country | Link |
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| CN (1) | CN117779163A (en) |
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2023
- 2023-12-27 CN CN202311829184.8A patent/CN117779163A/en active Pending
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