CN107699899B - Full-automatic polishing system and method for chemical buffering of whole surface of superconducting cavity - Google Patents
Full-automatic polishing system and method for chemical buffering of whole surface of superconducting cavity Download PDFInfo
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- CN107699899B CN107699899B CN201711006578.8A CN201711006578A CN107699899B CN 107699899 B CN107699899 B CN 107699899B CN 201711006578 A CN201711006578 A CN 201711006578A CN 107699899 B CN107699899 B CN 107699899B
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- 238000005498 polishing Methods 0.000 title claims abstract description 91
- 239000000126 substance Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000003139 buffering effect Effects 0.000 title claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 244
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 41
- 239000012498 ultrapure water Substances 0.000 claims abstract description 41
- 238000002156 mixing Methods 0.000 claims abstract description 40
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims description 84
- 238000002955 isolation Methods 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 24
- 239000000523 sample Substances 0.000 claims description 23
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 14
- 238000007517 polishing process Methods 0.000 claims description 13
- 239000007921 spray Substances 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 238000011010 flushing procedure Methods 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 6
- 239000000498 cooling water Substances 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 230000000007 visual effect Effects 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000005530 etching Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/08—Apparatus, e.g. for photomechanical printing surfaces
Abstract
The invention relates to the technical field of processing of superconducting cavities of ion accelerators, in particular to a full-automatic polishing system and method for chemical buffering of the whole cavity surface of a superconducting cavity. The device is characterized by comprising an acid mixing tank, wherein the upper end of the acid mixing tank is connected with a refrigerating unit through a pipeline, a heat exchanger is arranged in the acid mixing tank, the lower end of the acid mixing tank is connected with an acid liquor conveying pump through a pipeline, the acid liquor conveying pump is connected with a filter through a pipeline, the filter is connected with the lower end of a superconducting cavity and an ultrapure water pump through a pipeline, the ultrapure water pump is connected with an ultrapure water tank through a pipeline, the upper end of the superconducting cavity is respectively connected with the upper end of the acid mixing tank and an observation window through a pipeline, and a high-purity nitrogen tank is connected with a pipeline between the acid mixing tank and the superconducting cavity through a pipeline; the chemical buffer polishing of the multi-type superconducting cavity can be realized by strictly controlling the flow, the flow rate, the temperature, the pressure and the time of the acid liquor by adopting a computer. And has strong corrosion resistance, high safety, reliability, controllability and easy operability.
Description
Technical Field
The invention relates to the technical field of processing of superconducting cavities of ion accelerators, in particular to a full-automatic polishing system and method for chemical buffering of the whole cavity surface of a superconducting cavity.
Background
After the superconducting cavity is processed, the inner surface of the cavity must be polished, and in order to achieve the purpose of chemical buffer polishing, a set of system capable of realizing polishing operation needs to be developed, and meanwhile, a corresponding polishing medium needs to be provided. Because the superconducting cavity chemical polishing process adopts the highly toxic and highly corrosive mixed acid solution, the developed equipment must fully consider the personal safety of operators and equipment safety. In addition, the flow rate, the temperature, the pressure and the time of the acid liquid are strictly controlled in the working process of the equipment, so the equipment has to have strong corrosion resistance, high safety, reliability, controllability and easy operation.
The surface treatment methods commonly used at present are chemical buffer polishing, electrochemical polishing, plasma polishing, mechanical polishing and the like. And chemical buffer polishing is a widely applied superconducting cavity surface treatment technology. The chemical buffer polishing is to use mixed acid solution of hydrofluoric acid, nitric acid and phosphoric acid with a certain proportion to strip the inner surface of the niobium superconducting cavity by controlling the temperature so as to remove an oxide layer on the surface of the material and micro damage generated in machining. The chemical buffer polishing equipment in the prior art has single use object, poor safety and poor reliability.
Disclosure of Invention
The invention aims to provide a full-automatic chemical buffer polishing system and method for the whole cavity surface of a superconducting cavity, aiming at the defects of the prior art. Thereby effectively solving the problems in the prior art.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the full-automatic polishing system for the chemical buffering of the whole surface of the superconducting cavity is characterized by comprising an acid mixing tank, wherein the upper end of the acid mixing tank is connected with a refrigerating unit through a pipeline, a heat exchanger is arranged in the acid mixing tank, the lower end of the acid mixing tank is connected with an acid liquor conveying pump through a pipeline, the acid liquor conveying pump is connected with a filter through a pipeline, the filter is connected with the lower end of the superconducting cavity and an ultrapure water pump through a pipeline, the ultrapure water pump is connected with an ultrapure water tank through a pipeline, the upper end of the superconducting cavity is respectively connected with the upper end of the acid mixing tank and an observation window through a pipeline, and a high-purity nitrogen tank is connected with a pipeline between the acid mixing tank and the superconducting cavity through a pipeline.
A cold water valve is arranged on a pipeline between the mixed acid tank of the polishing equipment and the refrigerating unit; the mixed acid tank is provided with a second liquid level meter probe and a temperature probe, a pipeline between the acid liquid conveying pump and the filter is sequentially provided with a flowmeter and an acid supply valve, and the acid liquid conveying pump, the first stirring valve and the second stirring valve form a mixed acid circulation loop of the mixed acid tank through the pipeline; a third isolation valve, an acid return valve, a pressure sensor and a second isolation valve are sequentially arranged on the pipelines at the upper end of the acid mixing tank and the upper end of the superconducting cavity; the upper end of the high-purity nitrogen tank is connected with a pipeline between the pressure sensor and the second isolation valve through an output pipeline, and a gas high-pressure valve and a nitrogen control valve are arranged on the output pipeline of the high-purity nitrogen tank; the device comprises a superconducting cavity, a first liquid level meter probe, a liquid level control valve, a cavity liquid inlet valve, a discharge valve, a cooling spray valve, a first isolation valve and a cooling spray valve, wherein the first liquid level meter probe is arranged on the observation window; an acid inlet valve is arranged on a pipeline at the upper end of the filter, and a pure water valve is arranged on a pipeline at the front end of the ultrapure water pump; the pipeline between the acid return valve and the third isolation valve is connected with one end of the circulating valve through a pipeline, and the other end of the circulating valve is connected between the first stirring valve and the first isolation valve through a pipeline.
The full-automatic chemical buffer polishing method for the whole cavity surface of the superconducting cavity is characterized by comprising the following steps of:
(1) Parameter initialization: setting parameters of flow rate, temperature, polishing time, ultrapure water washing times and flushing time of the acid liquor polished by the cavity according to different cavity types in a computer;
(2) And (3) cavity pressure maintaining: filling ultrapure water into the superconducting cavity and applying 0-1.5 atmospheres to check whether leakage hidden trouble exists in the cavity, the pipeline connected with the cavity and the joint;
(3) Acid liquor circulation and temperature control: mixing, stirring and controlling the temperature of the needed different kinds of high-risk and high-corrosiveness acid liquor in the acid mixing tank to ensure that the acid liquor is fully fused; the mixed acid tank is used for realizing circulating stirring of mixed acid through an acid mixing loop formed by an acid liquid conveying pump, a first stirring valve and a second stirring valve; the acid liquor is added according to the volume ratio of 2:1:1 of phosphoric acid, nitric acid and hydrofluoric acid, and the acid liquor is circularly stirred for 5 minutes after the acid liquor is added; when the temperature of the acid liquor is higher and does not reach the working temperature, the computer starts the refrigerating unit to cool the acid liquor;
(4) Acid injection polishing of the cavity: when the acid liquor reaches the set temperature, the acid liquor conveying pump conveys the mixed acid liquor to the superconducting cavity through the corresponding pipeline and valve to realize the chemical polishing of the superconducting cavity, in the chemical polishing process, the pressure, the temperature, the flow and the polishing time of the liquid passing through the superconducting cavity are all monitored and controlled in real time by a computer, if various problems occur in the polishing, the control loop rapidly gives out an audible and visual alarm signal, and the fault position and the attribute are pointed out in a computer screen;
(5) Acid removal and cleaning: and after the polishing is finished, the acid liquor in the pipeline and the superconducting cavity is pumped back to the mixed acid tank by high-purity nitrogen through the corresponding pipeline and the valve, the acid liquor is recovered, the ultrapure water loop is started to wash and rinse the residual acid liquor in the cavity, and after washing for a plurality of times and for a certain time, the whole chemical buffer polishing process is finished.
The temperature control in the step (3) is realized by reading the data of the temperature probe by a computer so as to control a refrigerating unit, an acid liquid conveying pump and corresponding valves, and the temperature control is in the range of 0-30 ℃; the acid temperature control is carried out in two completely independent systems, one is a refrigerating unit, a heat exchanger and a valve, and the other is a mixed acid tank, an acid liquid conveying pump and related valves; the cooling water generated by the refrigerating unit circulates in the heat exchanger immersed in the acid liquid, the acid liquid in the mixed acid tank simultaneously circulates automatically, the temperature of the acid liquid is reduced by the contact between the surface of the heat exchanger and the acid liquid, and the temperature control of the acid liquid before polishing and the heat acid liquid generated in the chemical reaction in polishing is realized; the computer controls the temperature of the acid liquor in real time, and cold water generated by the refrigerating unit is circulated in the capillary cooler of the heat exchanger and the acid liquor is circulated to realize temperature exchange. After the temperature is lower than the set temperature, the temperature probe transmits a signal to the computer, the computer controls the refrigerating unit to stop working and closes the cold water valve, and the refrigerating process is repeated after the acid temperature rises. When the temperature of the acid liquor cannot be reduced to the required temperature through cooling, a cooling spray valve can be opened, and cooling water is sprayed onto the cavity through a spray head to reduce the temperature.
The cavity acid injection polishing process of the superconducting cavity in the step (4) comprises the following steps: starting an acid liquor conveying pump, performing acid liquor circulation temperature adjustment through a first stirring valve, a circulation valve and a third isolation valve, closing the valves after the acid liquor reaches a set temperature, starting polishing timing by a computer, and simultaneously opening an acid supply valve, an acid inlet valve, a cavity liquid inlet valve, a second isolation valve, an acid return valve and the third isolation valve, wherein the acid liquor returns to the acid mixing tank through the valves, a filter and a superconducting cavity, and performing reciprocating circulation on the acid liquor to realize surface etching of the superconducting cavity; stopping an acid liquid conveying pump by a computer after finishing polishing timing, closing an acid supply valve, an acid inlet valve and an acid return valve, opening a high-purity nitrogen control valve, and pressing acid liquid in a polishing cavity and a pipeline back to an acid mixing tank by nitrogen through a second isolation valve, a superconducting cavity, a circulation valve and a third isolation valve, so that cavity polishing is finished; the superconducting cavity is required to be subjected to heavy polishing and light polishing for two times, wherein the inner surface of the cavity is polished to 120 mu m in the heavy polishing process, then high-temperature annealing is carried out, and the annealing is carried out, and then the light polishing is carried out to remove 20 mu m; the polishing medium used for polishing was 40% hydrofluoric acid, 68% nitric acid and 85% phosphoric acid, which were mixed at a volume ratio of 1:1:2, and the acid temperature at the time of heavy polishing was controlled at 18℃and the acid temperature at the time of light polishing was controlled at 11 ℃.
The washing in the step (5) is carried out by washing with ultrapure water for five times and 10 minutes, and is specifically divided into: and (3) washing: starting an ultrapure water pump, pumping the ultrapure water from the ultrapure water tank, passing through a pure water valve, a cavity liquid inlet valve, a superconducting cavity and a liquid level control valve, when a first liquid level meter probe senses that liquid flows in an observation window, feeding back a liquid feedback signal to a computer, closing the pure water valve and the pure water pump by the computer, opening a first isolation valve and a discharge valve, discharging the cleaned wastewater, and repeating for five times to finish washing; flushing: after the washing is finished, the ultra-pure water is washed, and the washed waste water is discharged through a pure water valve, a cavity liquid inlet valve, a superconducting cavity, a washing valve and a discharge valve.
The beneficial effects of the invention are as follows: the full-automatic chemical buffer polishing system and method for the whole surface of the superconducting cavity can realize the chemical buffer polishing of the superconducting cavities with multiple types by strictly controlling the flow, the flow speed, the temperature, the pressure and the time of the acid liquor by adopting a computer. And has strong corrosion resistance, high safety, reliability, controllability and easy operability.
Description of the drawings:
FIG. 1 is a schematic diagram of the structure of the present invention;
fig. 2 is a schematic of the workflow of the present invention.
The figure shows: 1. an acid supply valve; 2. an acid inlet valve; 3. a pure water valve; 4. a first stirring valve; 5. a first isolation valve; 6. a cavity liquid inlet valve; 7. a second stirring valve; 8. a circulation valve; 9. a second isolation valve; 10. an acid return valve; 11. a liquid level control valve; 12. a third isolation valve; 13. a cold water valve; 14. a nitrogen control valve; 15. a gas high pressure valve; 16. a flush valve; 17. a discharge valve; 18. an acid liquid conveying pump; 19. a filter; 20. a superconducting cavity; 21. an observation window; 22. a refrigerating unit; 23. a mixed acid tank; 24. a heat exchanger; 25. a high purity nitrogen tank; 26. cooling the spray valve; 27. a first level gauge probe; 28. a second level gauge probe; 29. a temperature probe; 30. a flow meter; 31. a pressure sensor; 32. an ultrapure water pump; 33. ultrapure water tank; 34. a hydrofluoric acid detector; 35. and a nitric acid detector.
Detailed Description
The following is a further detailed description of the best mode examples illustrated in the accompanying drawings:
as shown in figure 1, the full-automatic polishing system for chemical buffering of the whole cavity surface of the superconducting cavity is characterized by comprising polishing equipment and a control system; the polishing device comprises an acid mixing tank 23, the upper end of the acid mixing tank 23 is connected with a refrigerating unit 22 through a pipeline, a heat exchanger 24 is arranged in the acid mixing tank 23, the lower end of the acid mixing tank 23 is connected with an acid liquid conveying pump 18 through a pipeline, the acid liquid conveying pump 18 is connected with a filter 19 through a pipeline, the filter 19 is connected with the lower end of a superconducting cavity 20 and an ultrapure water pump 32 through a pipeline, the ultrapure water pump 32 is connected with an ultrapure water tank 33 through a pipeline, the upper end of the superconducting cavity 20 is respectively connected with the upper end of the acid mixing tank 23 and an observation window 21 through a pipeline, and a high-purity nitrogen tank 25 is connected with a pipeline between the acid mixing tank 23 and the superconducting cavity 20 through a pipeline; the control system comprises a PLC industrial control computer and a relay circuit, wherein the PLC industrial control computer is used for realizing setting and adjusting of corresponding parameters of a polishing work site and realizing real-time control and display of a polishing process.
Further, a cold water valve 13 is arranged on a pipeline between the mixed acid tank 23 of the polishing device and the refrigerating unit 22; the mixed acid tank 23 is provided with a second liquid level meter probe 28 and a temperature probe 29, a flow meter 30 and an acid supply valve 1 are sequentially arranged on a pipeline between the acid liquid conveying pump 18 and the filter 19, and the acid liquid conveying pump 18, the first stirring valve 4 and the second stirring valve 7 form a mixed acid circulation loop of the mixed acid tank 23 through pipelines; a third isolation valve 12, an acid return valve 10, a pressure sensor 31 and a second isolation valve 9 are sequentially arranged on the pipelines at the upper end of the mixed acid tank 23 and the upper end of the superconducting cavity 20; the upper end of the high-purity nitrogen tank 25 is connected with a pipeline between the pressure sensor 31 and the second isolation valve 9 through an output pipeline, and a gas high-pressure valve 15 and a nitrogen control valve 14 are arranged on the output pipeline of the high-purity nitrogen tank 25; the observation window 21 is provided with a first liquid level meter probe 27, a liquid level control valve 11 is arranged on a pipeline connected with the upper end of the superconducting cavity 20 at the lower end of the observation window 21, a cavity liquid inlet valve 6 is arranged on the pipeline at the lower end of the superconducting cavity 20, the lower end of the superconducting cavity 20 is connected with a discharge valve 17 through a pipeline provided with a first isolation valve 5, the upper end of the superconducting cavity 20 is connected with the discharge valve 17 through a pipeline provided with a flushing valve 16, and a cooling spray valve 26 is arranged on a cooling pipeline at the upper part of the superconducting cavity 20; an acid inlet valve 2 is arranged on a pipeline at the upper end of the filter 19, and a pure water valve 3 is arranged on a pipeline at the front end of the ultrapure water pump 32; the pipeline between the acid return valve 10 and the third isolation valve 12 is connected with one end of the circulation valve 8 through a pipeline, and the other end of the circulation valve 8 is connected with the space between the first stirring valve 4 and the first isolation valve 5 through a pipeline.
Further, the control system controls an acid pump, a water pump, a valve, flow and a water cooling unit in the polishing equipment, acquires liquid level, temperature and pressure data, writes all operation data into a computer before each equipment operation, executes driving of corresponding equipment and devices by software operation, acquires signal data to perform corresponding operation, and records operation data and alarm records; the polishing equipment is also provided with a hydrofluoric acid detector 34 and a nitric acid detector 35, the hydrofluoric acid detector 34 and the nitric acid detector 35 are connected with a computer, and when the concentration of hydrofluoric acid and nitric acid in the field reaches a defined threshold value, the computer sends out an audible and visual alarm signal and gives a prompt in a screen.
As shown in FIG. 2, the full-automatic chemical buffer polishing method for the whole cavity surface of the superconducting cavity is characterized by comprising the following steps:
(1) Parameter initialization: setting parameters of flow rate, temperature, polishing time, ultrapure water washing times and flushing time of the acid liquor polished by the cavity according to different cavity types in a computer;
(2) And (3) cavity pressure maintaining: filling ultrapure water into the superconducting cavity and applying 0-1.5 atmospheres to check whether leakage hidden trouble exists in the cavity, the pipeline connected with the cavity and the joint;
(3) Acid liquor circulation and temperature control: mixing, stirring and controlling the temperature of the needed different kinds of high-risk and high-corrosiveness acid liquor in the acid mixing tank to ensure that the acid liquor is fully fused; the mixed acid tank 23 realizes the circulation stirring of mixed acid through a mixed acid loop formed by the acid liquid conveying pump 18, the first stirring valve 4 and the second stirring valve 7; the acid liquor is added according to the volume ratio of 2:1:1 of phosphoric acid, nitric acid and hydrofluoric acid, and the acid liquor is circularly stirred for 5 minutes after the acid liquor is added; when the temperature of the acid liquor is higher and does not reach the working temperature, the computer starts the refrigerating unit to cool the acid liquor;
(4) Acid injection polishing of the cavity: when the acid liquor reaches the set temperature, the acid liquor conveying pump conveys the mixed acid liquor to the superconducting cavity through the corresponding pipeline and valve to realize the chemical polishing of the superconducting cavity, in the chemical polishing process, the pressure, the temperature, the flow and the polishing time of the liquid passing through the superconducting cavity are all monitored and controlled in real time by a computer, if various problems occur in the polishing, the control loop rapidly gives out an audible and visual alarm signal, and the fault position and the attribute are pointed out in a computer screen;
(5) Acid removal and cleaning: and after the polishing is finished, the acid liquor in the pipeline and the superconducting cavity is pumped back to the mixed acid tank by high-purity nitrogen through the corresponding pipeline and the valve, the acid liquor is recovered, the ultrapure water loop is started to wash and rinse the residual acid liquor in the cavity, and after washing for a plurality of times and for a certain time, the whole chemical buffer polishing process is finished.
The temperature control in the step (3) is realized by reading the data of the temperature probe by a computer so as to control a refrigerating unit, an acid liquid conveying pump and corresponding valves, and the temperature control is in the range of 0-30 ℃; the acid temperature control is carried out in two completely independent systems, one is a refrigerating unit, a heat exchanger and a valve, and the other is a mixed acid tank 23, an acid liquid conveying pump 18 and related valves; the cooling water generated by the refrigerating unit circulates in the heat exchanger immersed in the acid liquid, the acid liquid in the mixed acid tank 23 simultaneously circulates automatically, the temperature of the acid liquid is reduced by the contact between the surface of the heat exchanger 24 and the acid liquid, and the temperature control of the acid liquid before polishing and the thermal acid liquid generated in the chemical reaction in polishing is realized; the computer will control the temperature of the acid in real time, and the cold water generated by the refrigerating unit 22 is circulated through the capillary cooler of the heat exchanger 24 and the acid to realize temperature exchange. After the temperature is lower than the set temperature, the temperature probe transmits a signal to the computer, and the computer controls the refrigerating unit 22 to stop working and closes the cold water valve 13, and the refrigerating process is repeated after the acid temperature rises. When the acid liquor cooling can not reduce the temperature to the required temperature, the cooling spray valve 26 can be opened, and cooling water is sprayed onto the cavity through the spray head to reduce the temperature.
The cavity acid injection polishing process of the superconducting cavity in the step (4) comprises the following steps: starting an acid liquor conveying pump 18, carrying out acid liquor circulation temperature adjustment through a first stirring valve 4, a circulation valve 8 and a third isolation valve 12, closing the valves after the acid liquor reaches a set temperature, starting polishing timing by a computer, and simultaneously opening an acid supply valve 1, an acid inlet valve 2, a cavity liquid inlet valve 6, a second isolation valve 9, an acid return valve 10 and the third isolation valve 12, wherein the acid liquor returns to an acid mixing tank 23 through the valves, a filter 19 and a superconducting cavity 20, and carrying out reciprocating circulation on the acid liquor to realize surface etching of the superconducting cavity; stopping the acid liquid conveying pump 18 by the computer after finishing polishing timing, closing the acid supply valve 1, the acid inlet valve 2 and the acid return valve 10, opening the high-purity nitrogen control valve 14, and pressing the acid liquid in the cavity and the pipeline in polishing back to the acid mixing tank by nitrogen through the second isolation valve 9, the superconducting cavity 20, the circulation valve 8 and the third isolation valve 12 to finish the cavity polishing; the superconducting cavity is required to be subjected to heavy polishing and light polishing for two times, wherein the inner surface of the cavity is polished to 120 mu m in the heavy polishing process, then high-temperature annealing is carried out, and the annealing is carried out, and then the light polishing is carried out to remove 20 mu m; the polishing medium used for polishing was 40% hydrofluoric acid, 68% nitric acid and 85% phosphoric acid, which were mixed at a volume ratio of 1:1:2, and the acid temperature at the time of heavy polishing was controlled at 18℃and the acid temperature at the time of light polishing was controlled at 11 ℃.
The washing in the step (5) is carried out by washing with ultrapure water for five times and 10 minutes, and is specifically divided into: and (3) washing: starting the ultrapure water pump 32, pumping the ultrapure water from the ultrapure water tank 33, passing through the pure water valve 3, the cavity liquid inlet valve 6, the superconducting cavity 20 and the liquid level control valve 11, and when the first liquid level meter probe 27 senses that the observation window 21 has liquid flowing in, feeding back a liquid feedback signal to a computer, closing the pure water valve 3 and the pure water pump by the computer, opening the first isolation valve 5 and the discharge valve 17 to discharge the cleaned wastewater, and repeating the steps for five times to finish the washing; flushing: after the washing, the ultra-pure water is washed, and the washed waste water is discharged through the pure water valve 3, the cavity liquid inlet valve 6, the superconducting cavity 20, the washing valve 16 and the discharge valve 17.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (3)
1. The full-automatic chemical buffer polishing method for the whole cavity surface of the superconducting cavity is characterized by comprising the following steps of:
(1) Parameter initialization: setting parameters of flow rate, temperature, polishing time, ultrapure water washing times and flushing time of the acid liquor polished by the cavity according to different cavity types in a computer;
(2) And (3) cavity pressure maintaining: after filling ultrapure water into the superconducting cavity, applying 1.5 atmospheres to check whether leakage hidden danger exists in the cavity, a pipeline connected with the cavity and a joint;
(3) Acid liquor circulation and temperature control: mixing, stirring and controlling the temperature of the needed different kinds of high-risk and high-corrosiveness acid liquor in the acid mixing tank to ensure that the acid liquor is fully fused; the mixed acid tank is used for realizing circulating stirring of mixed acid through an acid mixing loop formed by an acid liquid conveying pump, a first stirring valve and a second stirring valve; the acid liquor is added according to the volume ratio of 2:1:1 of phosphoric acid, nitric acid and hydrofluoric acid, and the acid liquor is circularly stirred for 5 minutes after the acid liquor is added; when the temperature of the acid liquor is higher and does not reach the working temperature, the computer starts the refrigerating unit to cool the acid liquor;
(4) Acid injection polishing of the cavity: when the acid liquor reaches the set temperature, the acid liquor conveying pump conveys the mixed acid liquor to the superconducting cavity through the corresponding pipeline and valve to realize the chemical polishing of the superconducting cavity, in the chemical polishing process, the pressure, the temperature, the flow and the polishing time of the liquid passing through the superconducting cavity are all monitored and controlled in real time by a computer, if various problems occur in the polishing, the control loop rapidly gives out an audible and visual alarm signal, and the fault position and the attribute are pointed out in a computer screen;
the cavity of the superconducting cavity is filled with acid and polished: starting an acid liquor conveying pump, performing acid liquor circulation temperature adjustment through a first stirring valve, a circulation valve and a third isolation valve, closing the valves after the acid liquor reaches a set temperature, starting polishing timing by a computer, and simultaneously opening an acid supply valve, an acid inlet valve, a cavity liquid inlet valve, a second isolation valve, an acid return valve and the third isolation valve, wherein the acid liquor returns to the acid mixing tank through the valves, a filter and a superconducting cavity, and performing reciprocating circulation on the acid liquor to realize surface etching of the superconducting cavity; stopping an acid liquid conveying pump by a computer after finishing polishing timing, closing an acid supply valve, an acid inlet valve and an acid return valve, opening a high-purity nitrogen control valve, and pressing acid liquid in a polishing cavity and a pipeline back to an acid mixing tank by nitrogen through a second isolation valve, a superconducting cavity, a circulation valve and a third isolation valve, so that cavity polishing is finished; the superconducting cavity is required to be subjected to heavy polishing and light polishing for two times, wherein the inner surface of the cavity is polished to 120 mu m in the heavy polishing process, then high-temperature annealing is carried out, and the annealing is carried out, and then the light polishing is carried out to remove 20 mu m; the polishing medium used for polishing was 40% hydrofluoric acid, 68% nitric acid and 85% phosphoric acid, which were mixed at a volume ratio of 1:1:2, with the acid temperature at the time of heavy polishing being 18 ℃ and the acid temperature at the time of light polishing being 11 ℃;
(5) Acid removal and cleaning: the polished acid liquor in the pipeline and the superconducting cavity is pumped back to the mixed acid tank by high-purity nitrogen through the corresponding pipeline and valve, after the acid liquor is recovered, the ultrapure water loop is started to wash and rinse the residual acid liquor in the cavity, and after washing for a plurality of times and for a certain time, the whole chemical buffer polishing process is completed;
the polishing system adopting the full-automatic polishing method for chemical buffering of the whole surface of the superconducting cavity comprises an acid mixing tank, wherein the upper end of the acid mixing tank is connected with a refrigerating unit through a pipeline, a heat exchanger is arranged in the acid mixing tank, the lower end of the acid mixing tank is connected with an acid liquor conveying pump through a pipeline, the acid liquor conveying pump is connected with a filter through a pipeline, the filter is connected with the lower end of the superconducting cavity and an ultrapure water pump through a pipeline, the ultrapure water pump is connected with an ultrapure water tank through a pipeline, the upper end of the superconducting cavity is respectively connected with the upper end of the acid mixing tank and an observation window through a pipeline, and a high-purity nitrogen tank is connected with a pipeline between the acid mixing tank and the superconducting cavity through a pipeline; a cold water valve is arranged on a pipeline between the mixed acid tank of the polishing equipment and the refrigerating unit; the mixed acid tank is provided with a second liquid level meter probe and a temperature probe, a pipeline between the acid liquid conveying pump and the filter is sequentially provided with a flowmeter and an acid supply valve, and the acid liquid conveying pump, the first stirring valve and the second stirring valve form a mixed acid circulation loop of the mixed acid tank through the pipeline; a third isolation valve, an acid return valve, a pressure sensor and a second isolation valve are sequentially arranged on the pipelines at the upper end of the acid mixing tank and the upper end of the superconducting cavity; the upper end of the high-purity nitrogen tank is connected with a pipeline between the pressure sensor and the second isolation valve through an output pipeline, and a gas high-pressure valve and a nitrogen control valve are arranged on the output pipeline of the high-purity nitrogen tank; the device comprises a superconducting cavity, a first liquid level meter probe, a liquid level control valve, a cavity liquid inlet valve, a discharge valve, a cooling spray valve, a first isolation valve and a cooling spray valve, wherein the first liquid level meter probe is arranged on the observation window; an acid inlet valve is arranged on a pipeline at the upper end of the filter, and a pure water valve is arranged on a pipeline at the front end of the ultrapure water pump; the pipeline between the acid return valve and the third isolation valve is connected with one end of the circulating valve through a pipeline, and the other end of the circulating valve is connected between the first stirring valve and the first isolation valve through a pipeline.
2. The full-automatic polishing method for chemical buffering of the whole surface of a superconducting cavity according to claim 1, wherein the method comprises the following steps: the temperature control in the step (3) is realized by reading data of a temperature probe by a computer so as to control a refrigerating unit, an acid liquid conveying pump and corresponding valves, and the temperature control is in the range of 0-30 ℃; the acid temperature control is carried out in two completely independent systems, one is a refrigerating unit, a heat exchanger and a valve, and the other is a mixed acid tank, an acid liquid conveying pump and related valves; the cooling water generated by the refrigerating unit circulates in the heat exchanger immersed in the acid liquid, the acid liquid in the mixed acid tank simultaneously circulates automatically, the temperature of the acid liquid is reduced by the contact between the surface of the heat exchanger and the acid liquid, and the temperature control of the acid liquid before polishing and the heat acid liquid generated in the chemical reaction in polishing is realized; the computer controls the temperature of the acid liquor in real time, and cold water generated by the refrigerating unit is circulated in a capillary cooler of the heat exchanger and the acid liquor is circulated to realize temperature exchange; after the temperature is lower than the set temperature, the temperature probe transmits a signal to the computer, the computer controls the refrigerating unit to stop working and closes the cold water valve, and the refrigerating process is repeated after the acid temperature rises; when the temperature of the acid liquor cannot be reduced to the required temperature through cooling, a cooling spray valve can be opened, and cooling water is sprayed onto the cavity through a spray head to reduce the temperature.
3. The full-automatic polishing method for chemical buffering of the whole surface of a superconducting cavity according to claim 1, wherein the method comprises the following steps: the washing in the step (5) is carried out by washing with ultrapure water for five times and 10 minutes, and is specifically divided into: and (3) washing: starting an ultrapure water pump, pumping the ultrapure water from the ultrapure water tank, passing through a pure water valve, a cavity liquid inlet valve, a superconducting cavity and a liquid level control valve, when a first liquid level meter probe senses that liquid flows in an observation window, feeding back a liquid feedback signal to a computer, closing the pure water valve by the computer, opening a first isolation valve and a discharge valve, and discharging the cleaned wastewater, and repeating for five times to finish washing; flushing: after the washing is finished, the ultra-pure water is washed, and the washed waste water is discharged through a pure water valve, a cavity liquid inlet valve, a superconducting cavity, a washing valve and a discharge valve.
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| CN109943851B (en) * | 2019-04-24 | 2021-04-27 | 中国科学院近代物理研究所 | Full-automatic polishing equipment for surface chemical buffering of superconducting cavity parts |
| CN111203410A (en) * | 2020-01-08 | 2020-05-29 | 中国科学院近代物理研究所 | Device and method for cleaning superconducting cavity |
| CN111800933B (en) * | 2020-07-08 | 2021-10-22 | 中国科学院高能物理研究所 | Medium-temperature annealing method for superconducting cavity |
| CN112870827A (en) * | 2020-12-30 | 2021-06-01 | 上海至纯洁净***科技股份有限公司 | Acid supply system for reducing generation of bubbles |
| CN113388872B (en) * | 2021-06-10 | 2022-11-15 | 中国科学院近代物理研究所 | Preparation method of composite-structure superconducting resonant acceleration cavity and superconducting resonant acceleration cavity |
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