CN220127014U - Graphite boat mixed liquid cleaning device - Google Patents
Graphite boat mixed liquid cleaning device Download PDFInfo
- Publication number
- CN220127014U CN220127014U CN202321026442.4U CN202321026442U CN220127014U CN 220127014 U CN220127014 U CN 220127014U CN 202321026442 U CN202321026442 U CN 202321026442U CN 220127014 U CN220127014 U CN 220127014U
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- CN
- China
- Prior art keywords
- liquid
- cleaning device
- graphite boat
- box body
- cleaning
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- 239000007788 liquid Substances 0.000 title claims abstract description 135
- 238000004140 cleaning Methods 0.000 title claims abstract description 81
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 45
- 239000010439 graphite Substances 0.000 title claims abstract description 45
- 230000005587 bubbling Effects 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 241000197194 Bulla Species 0.000 claims description 2
- 208000002352 blister Diseases 0.000 claims description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 7
- 230000009849 deactivation Effects 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 238000003475 lamination Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 21
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 10
- 239000011259 mixed solution Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 238000005507 spraying Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 238000005406 washing Methods 0.000 description 6
- 230000001502 supplementing effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
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- Detergent Compositions (AREA)
Abstract
The utility model relates to a graphite boat mixed liquid cleaning device, which comprises a mixed liquid device and a cleaning device, wherein the mixed liquid device is arranged above the cleaning device; the liquid mixing device comprises a liquid mixing box body, a liquid inlet and an air outlet are formed in the top of the liquid mixing box body, a liquid mixing outlet is formed in the bottom of the liquid mixing box body, the liquid mixing outlet is connected with one end of a liquid outlet pipeline, and a flowmeter is arranged on the liquid outlet pipeline; the top of the cleaning device is provided with an HF liquid inlet, and the bottom of the cleaning device is provided with a liquid adding opening and bubblingThe liquid adding port is connected with the other end of the liquid outlet pipeline, and the mixed liquid in the liquid mixing device is added into the cleaning device from the bottom of the cleaning device through the liquid outlet pipeline by utilizing pressure difference. The utility model can effectively clean SiOx/Poly-Si lamination removed by the graphite boat, achieve the purpose of complete deplating, and solve the problem of HCl+H 2 O 2 The problem of fast deactivation of the +HF cleaning system saves 20% HCl and 30% H 2 O 2 The dosage, after the complete deplating, the efficiency is improved to a certain extent compared with that before cleaning.
Description
Technical Field
The utility model relates to a cleaning device, in particular to a graphite boat mixed liquid cleaning device.
Background
In TOPCon cell production, a SiOx tunneling layer and a P-doped Poly-Si layer (TOPCon layer) are formed on the back surface, and the tube PECVD method is widely used as a mature technology. In the process of manufacturing the TOPCON layer, the graphite boat is used as a carrier to play a role of bearing and fixing a silicon wafer, the graphite boat is used after saturation is finished (one layer of silicon nitride is plated), an alternating layer structure of SiOx and P-doped Poly silicon is deposited outside the silicon nitride of the graphite boat in the production process, the alternating structure is gradually accumulated along with the increase of the using times of the graphite boat, and the coating quality is seriously affected when the alternating structure reaches a certain thickness, so that the graphite boat needs to be subjected to deplating after being recycled for a certain number of times, and the deplating is generally carried out by adopting a chemical cleaning method.
Currently, there are three main methods for cleaning graphite boats: and (3) cleaning the HNO3 and HF mixed solution, carrying out deplating on the saturated silicon nitride layer by high-concentration HF corrosion, and cleaning by high-concentration alkali (KOH/NaOH) after heating and cleaning by HF. The three methods are to directly prepare liquid in a cleaning tank and then to carry out circulating liquid replenishing.
The HNO3 method cleaning involves the problem of N emission, and the cleaning environment is more polluted; high concentration HF cleaning contains much floating, suspended and deposited Poly-Si, and continuous cleaning ability is poor; the alkaline cleaning is not thorough, high-frequency ignition can be formed, and the quality of the coating film is affected; therefore, all three methods have certain disadvantages.
Although HCl+H 2 O 2 The +HF mixed solution has strong cleaning capability, can achieve the aim of effective deplating, and has no pollution problem of nitrogen emission, but the cleaning of the formula is mainly due to the synergistic effect of HClO generated in the mixed solution and corrosion of Poly-Si and HF on SiOx, the HClO is easy to decompose, and simultaneously the HCl participating in the reaction is easy to volatilize and H 2 O 2 Is easy to decompose, and hardly plays a continuous and effective role in the long-time cleaning process, and the existing graphite boat cleaning device hardly plays a role in effectively using chemicals.
Disclosure of Invention
The utility model aims to solve the technical problems that: provides a graphite boat mixed liquid cleaning device which can effectively improve HCl and H 2 O 2 Is suitable for cleaning mixed liquid with gas generation.
The technical scheme adopted for solving the technical problems is as follows: the graphite boat mixed liquid cleaning device comprises a mixed liquid device and a cleaning device, wherein the mixed liquid device is arranged above the cleaning device; the liquid mixing device comprises a sealed and light-proof liquid mixing box body, a liquid inlet and an air outlet are formed in the top of the liquid mixing box body, a liquid mixing outlet is formed in the bottom of the liquid mixing box body, the liquid mixing outlet is connected with one end of a liquid outlet pipeline, and a flowmeter is arranged on the liquid outlet pipeline; the top of belt cleaning device be provided with HF inlet, belt cleaning device bottom be provided with liquid filling opening and tympanic bulla device, the other end of liquid outlet pipe is connected to the liquid filling opening, the mixed liquid in the mixed liquid device utilizes pressure differential to add to belt cleaning device in from the belt cleaning device bottom through the liquid outlet pipe.
Further, the mixed liquid box body is a PVDF box body or an FF box body or a PC box body.
Still further, the liquid inlet of the utility model comprises an HCL liquid inlet and H 2 O 2 A liquid inlet; the liquid inlet is provided with a liquid inlet pneumatic valve.
Still further, the exhaust port of the utility model is a normally open acid gas exhaust port.
Still further, the liquid adding openings are arranged in a row, and the liquid adding openings are separated from the bubbling device.
Still further, the bubbling device according to the present utility model is a nitrogen bubbling device.
The utility model has the beneficial effects that the defects existing in the background technology are overcome, the device can be used for effectively cleaning SiOx/Poly-Si lamination removed by a graphite boat, the purpose of complete deplating is achieved, and the mixed liquid cleaning device solves the problems of HCl+H 2 O 2 The problem of quick deactivation of the +HF cleaning system can save 20 percent of HCl and 30 percent of H compared with the direct liquid adding instead of liquid adding after liquid mixing 2 O 2 The dosage is as follows; the cleaning device is matched with HCl+H 2 O 2 The +HF is used for SiOx/Poly-Si cleaning, so that the pollution problem of nitrogen emission in nitric acid cleaning and the discontinuous problem of high-concentration HF cleaning are avoided, and the efficiency is improved to a certain extent after complete deplating compared with that before cleaning.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
in the figure: 1. a liquid mixing device; 2. a cleaning device; 11. a liquid mixing box body; 12. an HCL liquid inlet; 13. h 2 O 2 A liquid inlet; 14. an exhaust port; 15. a mixed liquid outlet; 16. a liquid outlet pipe; 17. a flow meter; 21. a liquid adding port; 22. a bubbling device; 23. HF liquid inlet.
Detailed Description
The utility model will now be described in further detail with reference to the drawings and a preferred embodiment. The drawings are simplified schematic representations which merely illustrate the basic structure of the utility model and therefore show only the structures which are relevant to the utility model.
The graphite boat mixed liquid cleaning device shown in fig. 1 comprises a mixed liquid device 1 and a cleaning device 2, wherein the mixed liquid device 1 is arranged above the cleaning device 2; the liquid mixing device comprises a sealed and opaque liquid mixing box 11, wherein the liquid mixing box 11 is a PVDF box or an FF box or a PC box.
The top of the liquid mixing box 11 is provided with a liquid inlet and an air outlet 14, and the liquid inlet comprises an HCL liquid inlet 12 and H 2 O 2 A liquid inlet 13; the liquid inlet is provided with a liquid inlet pneumatic valve; the exhaust port is a normally open acid gas exhaust port.
The bottom of the mixed liquor box 11 is provided with a mixed liquor outlet 15, the mixed liquor outlet is connected with one end of a liquor outlet pipeline 16, and a flowmeter 17 is arranged on the liquor outlet pipeline.
The top of the cleaning device 2 is provided with an HF liquid inlet 23, the bottom of the cleaning device is provided with a liquid adding port 21 and a bubbling device 22, the liquid adding port is arranged in a row, the liquid adding port is separated from the bubbling device, and the liquid is slowly bubbled at the same time of supplementing liquid, so that the supplemented mixed solution can be directly supplemented near the graphite boat to react with the SiOx/Poly-Si layer on the graphite boat, and the utilization rate of easily decomposed chemical substances in the mixed solution is greatly improved. The bubbling device is a nitrogen bubbling device. The liquid adding port is connected with the other end of the liquid outlet pipeline, and the mixed liquid in the liquid mixing device is added into the cleaning device from the bottom of the cleaning device through the liquid outlet pipeline by utilizing pressure difference.
According to the utility model, the mixed liquid is added into the cleaning tank after 8-10 minutes, and the utilization rate of HCl and H2O2 is improved by adding liquid at the bottom of the pressure difference, so that the generated HClO is directly reacted with the graphite boat, the mixed liquid contains Cl2, a certain water level pressure difference is kept, the mixed liquid is directly added into the mixed liquid tank from the bottom, and the liquid adding port has a certain bubbling function, so that the utilization rate of chemicals can be improved to the greatest extent.
The following is a detailed description of examples and comparative examples.
Examples
Firstly, placing a graphite boat into a primary solution, wherein the primary solution has a volume of 800L, 300L of 37% industrial hydrochloric acid, 100L of 30% hydrogen peroxide, 100L of 40% hydrofluoric acid and 300L of water are respectively added, a mixed solution and HF are added every 20min in a mode of liquid mixing and liquid supplementing, standing is carried out for 10 min after mixing, then the mixed solution is added into a graphite boat cleaning tank in a mode of liquid adding and liquid supplementing at the bottom, nitrogen bubbling is started at the same time, and then 3L of hydrofluoric acid is added, wherein the mixed solution is 4L of HL and 3L of H2O2. Experiments find that the graphite boat is cleaned in 50 min; secondly, taking out the graphite boat, putting the graphite boat into a washing tank, and spraying and cleaning for 30min; thirdly, placing the graphite boat into weak acid for bubbling cleaning for 1h after washing, wherein the proportion of the weak acid is as follows: 40% hydrofluoric acid 150L+37% hydrochloric acid 35L+600L water, and cleaning time is 30min; thirdly, spraying and cleaning the graphite boat after pickling for 30min; step four, rinsing for 240min by using clear water, wherein rinsing comprises spraying, bubbling and overflow functions; fifth step: slowly lifting and draining.
Comparative example 1 (direct addition of immiscible liquid)
In the first step, the graphite boat is put into a primary solution, wherein the primary solution has a volume of 800L, 300L of 37% industrial hydrochloric acid, 100L of 30% hydrogen peroxide, 100L of 40% hydrofluoric acid and 300L of water are respectively added, the primary solution is added for 20 minutes, and the added solution is 4L of hydrochloric acid, 3L of H2O2 and 3L of hydrofluoric acid respectively. In the cleaning method, the graphite boat is cleaned after 2 hours; secondly, taking out the graphite boat, putting the graphite boat into a washing tank, and spraying and cleaning for 30min; thirdly, placing the graphite boat into weak acid for bubbling cleaning for 1h after washing, wherein the proportion of the weak acid is as follows: 40% hydrofluoric acid 150L+37% hydrochloric acid 35L+600L water, and cleaning time is 30min; thirdly, spraying and cleaning the graphite boat after pickling for 30min; step four, rinsing for 240min by using clear water, wherein rinsing comprises spraying, bubbling and overflow functions; fifth step: slowly lifting and draining.
Comparative example 2 (mixing liquid and adding the mixture from the side)
Firstly, placing a graphite boat into a primary solution, wherein the primary solution has a volume of 800L, 300L of 37% industrial hydrochloric acid, 100L of 30% hydrogen peroxide, 100L of 40% hydrofluoric acid and 300L of water are respectively added, the mixed solution and HF are added every 20min in a mode of liquid mixing and liquid supplementing, the mixture is kept stand for 10 min after mixing, then the mixture is added into a graphite boat cleaning tank in a mode of liquid adding and liquid supplementing from the side, and then 3L of hydrofluoric acid is added, wherein the mixed solution is 4L of HL and 3L of H2O2. Experiments find that the graphite boat is cleaned after 1.5 hours; secondly, taking out the graphite boat, putting the graphite boat into a washing tank, and spraying and cleaning for 30min; thirdly, placing the graphite boat into weak acid for bubbling cleaning for 1h after washing, wherein the proportion of the weak acid is as follows: 40% hydrofluoric acid 150L+37% hydrochloric acid 35L+600L water, and cleaning time is 30min; thirdly, spraying and cleaning the graphite boat after pickling for 30min; step four, rinsing for 240min by using clear water, wherein rinsing comprises spraying, bubbling and overflow functions; fifth step: slowly lifting and draining.
The foregoing description is merely illustrative of specific embodiments of the utility model, and the utility model is not limited to the details shown, since modifications and variations of the foregoing embodiments may be made by those skilled in the art without departing from the spirit and scope of the utility model.
Claims (6)
1. A graphite boat mixes liquid belt cleaning device which characterized in that: the device comprises a liquid mixing device and a cleaning device, wherein the liquid mixing device is arranged above the cleaning device; the liquid mixing device comprises a sealed and light-proof liquid mixing box body, a liquid inlet and an air outlet are formed in the top of the liquid mixing box body, a liquid mixing outlet is formed in the bottom of the liquid mixing box body, the liquid mixing outlet is connected with one end of a liquid outlet pipeline, and a flowmeter is arranged on the liquid outlet pipeline; the top of belt cleaning device be provided with HF inlet, belt cleaning device's bottom be provided with liquid filling port and tympanic bulla device, the other end of liquid outlet pipe is connected to the liquid filling port, the mixed liquid in the mixed liquid device utilizes pressure differential to add to belt cleaning device in from the belt cleaning device bottom through the liquid outlet pipe.
2. The graphite boat liquid mixture cleaning device as set forth in claim 1, wherein: the mixed liquid box body is a PVDF box body or an FF box body or a PC box body.
3. The graphite boat liquid mixture cleaning device as set forth in claim 1, wherein: the liquid inlet comprises an HCL liquid inlet and H 2 O 2 A liquid inlet; the liquid inlet is provided with a liquid inlet pneumatic valve.
4. The graphite boat liquid mixture cleaning device as set forth in claim 1, wherein: the exhaust port is a normally open acid gas exhaust port.
5. The graphite boat liquid mixture cleaning device as set forth in claim 1, wherein: the liquid adding openings are arranged in a row, and the liquid adding openings are separated from the bubbling device.
6. The graphite boat liquid mixture cleaning device as set forth in claim 1, wherein: the bubbling device is a nitrogen bubbling device.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN202321026442.4U CN220127014U (en) | 2023-04-27 | 2023-04-27 | Graphite boat mixed liquid cleaning device |
Applications Claiming Priority (1)
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CN202321026442.4U CN220127014U (en) | 2023-04-27 | 2023-04-27 | Graphite boat mixed liquid cleaning device |
Publications (1)
Publication Number | Publication Date |
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CN220127014U true CN220127014U (en) | 2023-12-05 |
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CN202321026442.4U Active CN220127014U (en) | 2023-04-27 | 2023-04-27 | Graphite boat mixed liquid cleaning device |
Country Status (1)
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CN (1) | CN220127014U (en) |
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2023
- 2023-04-27 CN CN202321026442.4U patent/CN220127014U/en active Active
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