CN113707765A - Control method of surface treatment apparatus - Google Patents
Control method of surface treatment apparatus Download PDFInfo
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- CN113707765A CN113707765A CN202111005604.1A CN202111005604A CN113707765A CN 113707765 A CN113707765 A CN 113707765A CN 202111005604 A CN202111005604 A CN 202111005604A CN 113707765 A CN113707765 A CN 113707765A
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- 238000004381 surface treatment Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 164
- 239000007788 liquid Substances 0.000 claims abstract description 159
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 158
- 239000000243 solution Substances 0.000 claims abstract description 77
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000007599 discharging Methods 0.000 claims description 13
- 230000001502 supplementing effect Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 16
- 230000003647 oxidation Effects 0.000 abstract description 13
- 239000012535 impurity Substances 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 26
- 238000000354 decomposition reaction Methods 0.000 description 14
- 230000009286 beneficial effect Effects 0.000 description 13
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 9
- 229910017604 nitric acid Inorganic materials 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 238000005086 pumping Methods 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 229910021417 amorphous silicon Inorganic materials 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 2
- 239000003637 basic solution Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000861 blow drying Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic Table
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67017—Apparatus for fluid treatment
- H01L21/67063—Apparatus for fluid treatment for etching
- H01L21/67075—Apparatus for fluid treatment for etching for wet etching
- H01L21/67086—Apparatus for fluid treatment for etching for wet etching with the semiconductor substrates being dipped in baths or vessels
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/547—Monocrystalline silicon PV cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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- Microelectronics & Electronic Packaging (AREA)
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Abstract
The invention provides a control method of a surface treatment device, which comprises the following steps: s0: providing a reaction tank, a liquid circulation device and an ozone generation device, S1: communicating the liquid circulation device with the reaction tank, communicating the ozone generation device with the liquid circulation device, and S2: introducing a certain amount of hydrofluoric acid solution into the reaction tank, wherein the ratio of S3: starting the ozone generating device to generate ozone, starting the liquid circulating device to drive the solution in the reaction tank to enter the liquid circulating device, so that the solution entering the liquid circulating device is mixed with the ozone, and conveying the mixed solution back to the reaction tank, S4: and immersing the target object to be treated in the reaction tank for surface treatment, and taking out. The control method of the surface treatment equipment has simple treatment steps, does not generate impurities which can prevent oxidation and deoxidation, and has low cost.
Description
Technical Field
The invention relates to the technical field of solar energy, in particular to a control method of surface treatment equipment.
Background
The silicon substrate solar cell is characterized in that intrinsic and doped amorphous silicon layers are grown on the surface of a silicon wafer to form a special PN junction, and light energy can be converted into electric energy. The grown intrinsic and doped amorphous silicon layers are in the nanometer order, so that the intrinsic and doped amorphous silicon layers are very easy to be damaged in the preparation process, the electric leakage phenomenon is caused, and the efficiency and the reliability of the battery are reduced. Therefore, the surface of the pyramid structure after the texturing of the silicon wafer needs to be processed, so that the tips and edges of the pyramid structure are smoother, the thickness of the regrown amorphous silicon layer is more uniform, and the electric leakage caused by friction damage is not easy to occur.
The existing battery texturing main process comprises the following steps: pre-cleaning, rough polishing, water washing, texturing, cleaning, surface treatment (sharpening and corroding), cleaning and blow-drying. Chinese patent application publication No. CN106449373A discloses a method for etching and cleaning a heterojunction battery, in which a mixed solution of nitric acid and hydrofluoric acid is used to etch a silicon wafer during surface treatment, the nitric acid in the solution is used to oxidize the etched silicon wafer, and the hydrofluoric acid is used to remove an oxide layer, thereby achieving the effect of etching treatment. Because nitric acid can produce nitrous acid in the reaction process, so the reaction rate, poor stability and high liquid changing frequency are easily influenced, and a liquid inlet pipeline and a liquid discharge dilution pipeline of two kinds of acid liquor are required to be arranged at a tank device at the same time so as to discharge the mixed acid liquor with concentration which does not meet the requirements after the reaction for a period of time. In addition, a large amount of heat is generated when the surface treatment is performed using nitric acid, and a cryostat system is required to ensure the stability of the apparatus. It follows that this prior art method leads to a large amount of nitric acid and to complex and costly treatment steps.
Therefore, it is necessary to design a processing method with simple steps, easy use and low cost.
Disclosure of Invention
The invention aims to provide a control method of surface treatment equipment, which is used for solving the problems of complex surface treatment steps and high treatment cost in the prior art.
In order to achieve the above object, the present invention provides a surface treatment apparatus, comprising a reaction tank, an ozone generating device, a liquid inlet device, a liquid discharge device and a liquid circulating device, wherein the liquid inlet device and the liquid discharge device are both communicated with the reaction tank, the reaction tank is used for surface treatment of a target, the liquid inlet device is used for inputting liquid into the reaction tank, the liquid discharge device is used for discharging the liquid in the reaction tank, the ozone generating device is communicated with the liquid circulating device, the ozone generating device is used for generating ozone and conveying the ozone into the liquid circulating device, so that at least part of the ozone is dissolved in the liquid circulating device and forms a return liquid, the liquid circulating device is communicated with the reaction tank, and the liquid circulating device is used for pumping out part of the liquid in the reaction tank, and returning the reflux liquid to the reaction tank.
The surface treatment equipment has the beneficial effects that: the feed liquor device with drain all with the reaction tank intercommunication, the reaction tank is used for carrying out surface treatment to the target thing, feed liquor device be used for to input liquid in the reaction tank, drain is used for discharging the liquid in the reaction tank, ozone generating device with the liquid circulation device intercommunication, ozone generating device is used for producing ozone and will ozone is carried extremely in the liquid circulation device, makes at least part ozone dissolve with in the liquid circulation device and form backward flow liquid, liquid circulation device with the reaction tank intercommunication, liquid circulation device be used for with partial liquid in the reaction tank is taken out, and will backward flow liquid is carried back to the reaction tank. Adding a certain amount of hydrofluoric acid solution into the reaction tank, pumping the solution in the reaction tank into the liquid circulation device through the liquid circulation device, inputting ozone into the solution in the liquid circulation device through the ozone generation device to form a hydrofluoric acid solution dissolved with the ozone, conveying the hydrofluoric acid solution dissolved with the ozone back into the reaction tank under the continuous action of the liquid circulation device, oxidizing the surface of a silicon wafer through the dissolved ozone when a battery is treated, removing an oxidation layer through the hydrofluoric acid, decomposing the ozone into oxygen after reaction, diffusing the hydrofluoric acid to generate water and inorganic matters after the reaction, dissolving the generated water and the inorganic matters into the solution or precipitating at the bottom without generating impurities which can prevent oxidation and oxidation, and quantitatively discharging and supplementing the solution in the reaction tank through the liquid inlet device and the liquid discharge device, the concentration of the solution in the reaction tank can be ensured, and the battery can be treated without stopping the machine, so that the surface treatment equipment has the advantages that a liquid discharge dilution pipeline is not required to be arranged, the structure is simple, a large amount of manpower and material resources are not required to be consumed for treating the nitrogen-containing waste liquid, and the cost of a processing layer can be reduced; impurities which can interfere with the reaction can not be generated in the oxidation and deoxidation processes, so that the surface treatment of the battery is convenient; through the liquid inlet device with drain's cooperation can not shut down the processing, can promote machining efficiency.
In a feasible scheme, the system further comprises a temperature control device, wherein the temperature control device is arranged in the reaction tank and is used for acquiring the temperature of the reaction tank and regulating and controlling the temperature of the reaction tank. The beneficial effects are that: set up temperature control device can monitor and regulate and control temperature in the reaction tank is convenient for keep the stability of external conditions in oxidation and deoxidation process, is convenient for guarantee the normal clear of reaction process, and uses ozone oxidizes the battery, can not produce a large amount of heats, can simplify temperature control device's structure.
In one possible solution, the liquid circulation device comprises a first pipeline, a second pipeline and a circulation pump, two ends of the first pipeline are respectively communicated with the reaction tank and one end of the circulating pump, two ends of the second pipeline are respectively communicated with the reaction tank and the other end of the circulating pump, the circulating pump is used for pumping out the liquid in the reaction tank through the first pipeline and conveying the liquid to the reaction tank through the second pipeline, the ozone generating device comprises an ozone generator, a third pipeline and an ejector, wherein two ends of the third pipeline are respectively communicated with the ozone generator and the second pipeline, the ejector is arranged at the joint of the third pipeline and the second pipeline, the ozone generator is used for generating ozone and conveying the ozone to the third pipeline, the ejector is used for conveying the ozone in the third pipeline to the second pipeline. The beneficial effects are that: the circulating pump pumps the solution in the reaction tank into the circulating pump through the first pipeline, the solution in the circulating pump is continuously pumped back into the reaction tank through the second pipeline under the continuous action of the circulating pump, meanwhile, the ozone generator produces ozone and conveys the ozone into the third pipeline, the ejector conveys the ozone in the third pipeline into the second pipeline, the ozone can be dissolved in the solution in the second pipeline, the dissolution rate of the ozone can be improved compared with the mode of directly introducing the ozone into the reaction tank through the mode of dissolving the ozone outside the tank, the use efficiency of the ozone is improved, meanwhile, the ejector conveys the ozone into the second pipeline, and the proportion of the ozone flowing back to the ozone generator through the third pipeline can be reduced, assisting the ozone to enter the second pipeline.
In one possible embodiment, the ozone decomposition device is in communication with the second pipeline, and the ozone decomposition device is configured to decompose undissolved ozone. The beneficial effects are that: because the dissolution value of the ozone in water is limited, the ozone decomposition device can decompose the undissolved ozone through the ozone decomposition device, and the damage to workers caused by the direct discharge of the excessive ozone in the air is avoided.
In a feasible scheme, the second pipeline comprises a first section part, a second section part and a third section part which are sequentially communicated, the first section part is communicated with the circulating pump, the third section part is communicated with the reaction tank, the first section part and the third section part are vertically arranged, the second section part is horizontally arranged, the second section part is positioned on the top sides of the first section part and the third section part, and the ozone decomposition device is communicated with the second section part. The beneficial effects are that: set up like this and be convenient for promote to carry back in the reaction tank in the reflux liquid ozone's stability reduces ozone is in reaction tank department diffuses the volume in the atmosphere, utilizes gaseous density to be less than the density of water and passes through ozone decomposition device will gather in second section department ozone transports away, avoids gaseous piling up to block the circulation of second pipeline.
In a feasible scheme, the liquid circulation device further comprises a plurality of guide vanes, and the guide vanes are uniformly arranged on the inner side wall of the second pipeline. The beneficial effects are that: the guide vanes are arranged to enable the backflow liquid to rotate in the second pipeline, and the dissolving speed of the ozone can be improved.
In one possible embodiment, the angle between the guide vanes and the side wall of the second pipe is 20-70 °. The beneficial effects are that: the arrangement can improve the movement time of the ozone in the second pipeline and improve the dissolution time of the ozone.
The invention provides a control method of the surface treatment equipment, which comprises the following steps: s0: providing a reaction tank, a liquid circulation device and an ozone generation device, S1: communicating the liquid circulation device with the reaction tank, communicating the ozone generation device with the liquid circulation device, and S2: introducing a certain amount of hydrofluoric acid solution into the reaction tank, wherein the ratio of S3: starting the ozone generating device to generate ozone, starting the liquid circulating device to drive the solution in the reaction tank to enter the liquid circulating device, so that the solution entering the liquid circulating device is mixed with the ozone, and conveying the mixed solution back to the reaction tank, S4: and immersing the target object to be treated in the reaction tank for surface treatment, and taking out. The control method of the surface treatment equipment has the advantages that: the ozone generating device is used for generating ozone, the liquid circulating device is used for pumping out the hydrofluoric acid solution in the reaction tank and dissolving the ozone, then the hydrofluoric acid solution is conveyed back to the reaction tank, then the target object is immersed in the hydrogen fluoride solution dissolved with the ozone, the surface of the target object is oxidized by the ozone, and an oxide layer is removed by hydrofluoric acid, so that the treatment mode has simple steps, no impurities which hinder oxidation and oxidization removal are generated, the cost is low, and the liquid circulating device is used for dissolving the ozone outside the reaction tank, so that the utilization rate of the ozone is improved; compared with a mode of directly introducing ozone into the reaction tank, the mode is safer.
In a possible solution, the following steps are further included after the step S4: s5: providing an inlet means and a discharge means, S6: communicating the liquid inlet device and the liquid discharge device with the reaction tank respectively, and S7: and discharging a certain amount of solution through the liquid discharging device, and supplementing a certain amount of solution through the liquid inlet device. The beneficial effects are that: set up the inlet means with drain can not shut down and carry out the surface treatment of battery, promotes work efficiency.
In one possible embodiment, the concentration of the hydrofluoric acid solution in the step S2 is 0.5-1.5%. The beneficial effects are that: the concentration of the hydrofluoric acid solution is set to be 0.5-1.5%, on one hand, the hydrogen fluoride is convenient for performing deoxidation treatment on the oxidized target object, on the other hand, the reacted solution is also convenient for being directly discharged, the environment is protected, and the discharge process is simplified.
In a possible embodiment, the step S3 of mixing the solution entering the liquid circulation device with the ozone includes: controlling the ozone generating device to generate ozone at 150-3And at a flow rate of 5-50SLM into the liquid circulation means. The beneficial effects are that: the concentration of ozone dissolved in the solution in the second pipeline can be ensured by the arrangement, and the concentration of ozone in the reaction tank is ensured.
In one possible embodiment, in step S3, the concentration of ozone in the mixed solution is controlled to be 30-50 ppm. The beneficial effects are that: the reaction rate of the target in the solution can be accelerated, the processing efficiency is improved, and the cost is reduced.
In one possible embodiment, the step S4, after the target object to be processed is immersed in the reaction tank, includes the steps of: controlling the temperature in the reaction tank to be 25-30 ℃. The beneficial effects are that: the setting can guarantee the stability and the dissolution rate of the ozone, and meanwhile, the reaction heat of the ozone is small, so that the temperature is maintained, and in addition, the temperature can guarantee the normal operation of oxidation and deoxidation reactions.
In one possible embodiment, in the step S6, the volume of the certain amount of solution in the certain amount of solution is discharged by the liquid discharge device to be 0.5 to 10% of the volume of the solution in the reaction tank. The beneficial effects are that: the arrangement can ensure the concentration of the hydrogen fluoride solution in the reaction tank and can reduce the influence on oxidation and deoxidation reactions.
Drawings
FIG. 1 is a schematic view of a part of a surface treatment apparatus according to a first embodiment of the present invention;
FIG. 2 is a schematic view of the operation of the surface treating apparatus of FIG. 1;
FIG. 3 is a schematic view of the second duct and guide vanes of FIG. 1;
FIG. 4 is a schematic structural view of a reaction tank, a liquid inlet device, a liquid discharge device and a temperature control device according to a first embodiment of the present invention;
FIG. 5 is a schematic diagram of the liquid inlet device and the liquid discharge device in FIG. 4;
fig. 6 is a schematic view of a method of controlling the surface treatment apparatus according to the second embodiment of the present invention.
Reference numbers in the figures:
1. a reaction tank;
2. an ozone generating device; 201. an ozone generator; 202. a third pipeline;
3. a liquid inlet device; 301. a fourth pipeline; 302. a fifth pipeline; 303. an on-off valve; 304. a flow controller;
4. a liquid discharge device; 401. a sixth pipeline;
5. a liquid circulation device; 501. a first pipeline; 502. a second pipeline; 503. a circulation pump; 504. a first section; 505. a second section; 506. a third section; 507. a guide blade;
6. a temperature control device; 601. a seventh pipeline;
7. an ozone decomposing device.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. As used herein, the word "comprising" and similar words are intended to mean that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items.
The surface treatment mode among the prior art is usually carried out using nitric acid and hydrogen fluoride mixed acid, because nitric acid can produce nitrous acid in reaction process and influence reaction rate, and because the instability of nitric acid needs the liquid replacement fluid infusion process of higher frequency, nitric acid is the strong acid in addition, can not directly discharge during the emission, need set up the liquid discharge dilution pipeline and dilute the liquid of emission, can increase the complexity of device.
In view of the problems of the prior art, embodiments of the present invention provide a surface treatment apparatus.
Fig. 1 is a schematic view of a part of a surface treatment apparatus according to a first embodiment of the present invention, fig. 2 is a schematic view of an operating state of the surface treatment apparatus of fig. 1, fig. 4 is a schematic view of a reaction tank, a liquid inlet means, a liquid discharge means, and a temperature control means according to the first embodiment of the present invention, and fig. 5 is a schematic view of the liquid inlet means and the liquid discharge means of fig. 4.
In some embodiments of the present invention, referring to fig. 1, fig. 2 and fig. 4, the present invention comprises a reaction tank 1, an ozone generating device 2, a liquid inlet device 3, a liquid discharging device 4 and a liquid circulating device 5, wherein the liquid inlet device 3 and the liquid discharging device 4 are both communicated with the reaction tank 1, the reaction tank 1 is used for surface treatment of a target object, the liquid inlet device 3 is used for inputting liquid into the reaction tank 1, the liquid discharging device 4 is used for discharging the liquid in the reaction tank 1, the ozone generating device 2 is communicated with the liquid circulating device 5, the ozone generating device 2 is used for generating ozone and conveying the ozone into the liquid circulating device 5, so that at least part of the ozone is dissolved in the liquid circulating device 5 and forms a reflux liquid, the liquid circulating device 5 is communicated with the reaction tank 1, the liquid circulating device 5 is used for pumping out part of the liquid in the reaction tank 1, and the reflux liquid is sent back to the reaction tank 1.
In some embodiments of the present invention, referring to fig. 1, fig. 2, fig. 4 and fig. 5, a reaction tank 1 is a hollow box structure with an open top, a water inlet and a water outlet are formed in a side wall of the reaction tank 1, the liquid circulation device 5 is communicated with the water inlet and the water outlet, the ozone generation device 2 is disposed at one side of the liquid circulation device 5, the ozone generation device 2 is communicated with the liquid circulation device 5, the liquid inlet device 3 is disposed at an upper side of the reaction tank 1, the liquid inlet device 3 comprises a fourth pipeline 301 and a fifth pipeline 302, the liquid discharge device 4 comprises a sixth pipeline 401, the fourth pipeline 301, the fifth pipeline 302 and the sixth pipeline 401 are respectively provided with a switch valve 303 and a flow controller 304, the fourth pipeline 301 is used for introducing water into the reaction tank 1, the fifth pipeline 302 is used for introducing hydrogen fluoride into the reaction tank 1, a liquid discharge hole is formed in the side wall of the bottom of the reaction tank 1, the sixth pipeline 401 is communicated with the night-time air chamber, and the solution in the reaction tank 1 is discharged outwards through the sixth pipeline 401. During the use through inlet means 3 to add a certain amount of water and hydrogen fluoride in the reaction tank 1, form hydrogen fluoride solution, later open ozone generating device 2 with liquid circulating device 5 a period makes contain the ozone of certain density in the solution in the reaction tank 1, later in soak the target object of treating in the reaction tank 1, take out after the processing is accomplished, later put into next batch target object of treating and continue to carry out surface treatment. Along with the progress of the treatment process, the concentration of the hydrogen fluoride solution in the reaction tank 1 is gradually reduced, meanwhile, water and hydrogen fluoride with certain concentration are supplemented into the reaction tank 1 through the liquid inlet device 3, and the diluted hydrogen fluoride solution after the reaction in the reaction tank 1 is discharged through the liquid discharge device 4.
In some embodiments of the present invention, referring to fig. 4, the present invention further includes a temperature control device 6, the temperature control device 6 is disposed in the reaction tank 1, and the temperature control device 6 is configured to obtain the temperature of the reaction tank 1 and to regulate and control the temperature of the reaction tank 1.
In some embodiments of the present invention, referring to fig. 4 and 5, the temperature control device 6 includes a temperature sensor (not shown), a controller (not shown), a seventh pipeline 601 and a water pump (not shown), the temperature sensor is disposed in the reaction tank 1, the temperature sensor is used for measuring the temperature in the reaction tank 1, the seventh pipeline 601 is disposed at the bottom of the reaction tank 1, the seventh pipeline 601 is communicated with a water source, the water pump is disposed on the seventh pipeline 601, the temperature sensor and the water pump are both electrically connected to the controller, and the controller controls the on/off of the water pump according to the temperature of the reaction tank 1 measured by the temperature sensor. During the in-service use, the water source is the factory cooling water of temperature normal atmospheric temperature (temperature is not higher than 25 ℃), through the controller will the temperature regulation and control scope of reaction tank 1 sets up to 25-30 ℃, works as temperature sensor detects when the temperature of reaction tank 1 is located this within range, the controller control the water pump is closed, along with the going on of surface treatment process, the temperature in the reaction tank 1 can rise along with the emergence temperature of oxidation and deoxidation reaction gradually, works as temperature sensor detects when the temperature in the reaction tank 1 is higher than 30 ℃, the controller control the water pump is opened right reaction tank 1 cools down, works as after the temperature of reaction tank 1 falls back to 25-27 ℃ the controller control the water pump is closed. The arrangement can ensure that the temperature of the reaction tank 1 is in the range of 25-30 ℃, on one hand, the temperature rise is avoided to enable ozone to be directly diffused, on the other hand, the ambient temperature when the oxidation or deoxidation reaction is carried out can be ensured, the normal running of the reaction is convenient, and the speed and the effect of the oxidation and the deoxidation are ensured.
In some embodiments of the present invention, referring to fig. 1 and 2, the liquid circulation device 5 includes a first pipeline 501, a second pipeline 502 and a circulation pump 503, two ends of the first pipeline 501 are respectively communicated with one ends of the reaction tank 1 and the circulation pump 503, two ends of the second pipeline 502 are respectively communicated with the other ends of the reaction tank 1 and the circulation pump 503, the circulation pump 503 is used for pumping out the liquid in the reaction tank 1 through the first pipeline 501 and delivering the liquid to the reaction tank 1 through the second pipeline 502, the ozone generation device 2 includes an ozone generator 201, a third pipeline 202 and an ejector (not shown in the figure), two ends of the third pipeline 202 are respectively communicated with the ozone generator 201 and the second pipeline 502, the ejector is arranged at the connection position of the third pipeline 202 and the second pipeline 502, the ozone generator 201 is used for generating ozone and delivering the ozone to the third pipeline 202, and the ejector is used for delivering the ozone in the third pipeline 202 to the second pipeline 502.
In some embodiments of the present invention, the water outlet is disposed at the lower side of the water inlet, two ends of the first pipeline 501 are respectively communicated with the water outlet and one end of the circulating pump 503, two ends of the second pipeline 502 are respectively communicated with the water inlet and the other end of the circulating pump 503, the ozone generator 201 is a commercially available device for producing ozone, the ozone generator 201 is communicated with the second pipeline 502 through the third pipeline 202, the ejector (not shown) is a device that ejects air flow or liquid flow from a nozzle under the action of pressure, the ejector is disposed at the connection position of the third pipeline 202 and the second pipeline 502, the ozone generator 201 conveys the ozone into the third pipeline 202 and conveys the ozone into the second pipeline 502 under the action of the ejector, the ejector is arranged to assist the ozone to enter the second pipeline 502 on the one hand, and to prevent the solution in the second pipeline 502 from entering the third pipeline 202 on the other hand.
In some embodiments of the present invention, referring to fig. 2, further comprising an ozone decomposition device 7, wherein the ozone decomposition device 7 is in communication with the second pipeline 502, and the ozone decomposition device 7 is used for decomposing undissolved ozone.
In some embodiments of the present invention, the ozone decomposition device 7 is communicated with the second pipeline 502 through a pipeline, and an interface between the ozone decomposition device 7 and the second pipeline 502 is disposed on a side of the ejector away from the circulation pump 503, and the ozone decomposition device 7 extracts the undissolved ozone in the second pipeline 502 through a pipeline, processes the ozone into oxygen, and discharges the oxygen.
In some embodiments of the present invention, referring to fig. 2, the second pipeline 502 includes a first section 504, a second section 505 and a third section 506 which are sequentially communicated, the first section 504 is communicated with the circulation pump 503, the third section 506 is communicated with the reaction tank 1, the first section 504 and the third section 506 are both vertically arranged, the second section 505 is horizontally arranged, the second section 505 is located on the top sides of the first section 504 and the third section 506, and the ozone decomposition device 7 is communicated with the second section 505.
In some embodiments of the present invention, the first section 504 and the third section 506 are vertically disposed, the second section 505 is horizontally disposed on the top sides of the first section 504 and the third section 506, such that the gas in the second pipeline 502 is collected at the second pipeline 502, and the connection between the ozone decomposition device 7 and the second pipeline 502 is disposed at the second section 505, such that the undissolved gas is extracted.
In addition, the diameters of the first section 504, the second section 505 and the third section 506 are all 5-20CM, the length of the first section 504 is 40-150CM, the length of the second section 505 is 10-40CM, and the length of the third section 506 is 40-150 CM.
Fig. 3 is a schematic structural view of the second pipe and the guide vane in fig. 1.
In some embodiments of the present invention, referring to fig. 1 and 3, the liquid circulation device 5 further includes a plurality of guide vanes 507, and the guide vanes 507 are uniformly disposed on the inner side wall of the second pipeline 502.
In some embodiments of the present invention, referring to fig. 3, the plurality of guide vanes 507 are uniformly disposed on the inner sidewall of the second section 505, and the guide vanes 507 can improve the solubility of ozone.
It should be noted that the same effect can be achieved by replacing the guide vanes 507 with motor-driven helical vanes.
In some embodiments of the present invention, referring to fig. 3, the angle between the guide vane 507 and the sidewall of the second conduit 502 is 20-70 °.
In some embodiments of the present invention, the guiding vanes 507 are disposed along the flowing direction of the solution, and the angle between the guiding vanes 507 and the vertical direction is 36 °.
Fig. 6 is a schematic view of a method of controlling the surface treatment apparatus according to the second embodiment of the present invention.
In some embodiments of the present invention, referring to fig. 6, a method of controlling a surface treatment apparatus includes the steps of: s0: providing a reaction tank, a liquid circulation device and an ozone generation device, S1: communicating the liquid circulation device 5 with the reaction tank 1, communicating the ozone generation device 2 with the liquid circulation device 5, and S2: introducing a certain amount of hydrofluoric acid solution into the reaction tank 1, wherein the ratio of S3: starting the ozone generating device 2 to generate ozone, starting the liquid circulating device 5 to drive the solution in the reaction tank 1 to enter the liquid circulating device 5, so that the solution entering the liquid circulating device 5 is mixed with the ozone, and the mixed solution is conveyed back to the reaction tank 1, S4: and immersing the target object to be treated into the reaction tank 1 for surface treatment, and taking out.
In some embodiments of the present invention, the liquid circulation device 5 is communicated with the reaction tank 1, the ozone generation device 2 is communicated with the liquid circulation device 5, and the ozone generated by the ozone generation device 2 can be conveyed into the reaction tank 1 through the liquid circulation device 5; introducing a certain amount of hydrofluoric acid solution into the reaction tank 1, providing a basic solution for carrying out a deoxidation reaction, and providing the basic solution extracted by the liquid circulation device 5; starting the ozone generating device 2 to generate ozone, starting the liquid circulating device 5 to drive the solution in the reaction tank 1 to enter the liquid circulating device 5, so that the solution entering the liquid circulating device 5 is mixed with the ozone, conveying the mixed solution back to the reaction tank 1, and mixing the ozone produced by the ozone generating device into the hydrofluoric acid solution through the liquid circulating device 5; immersing a target object to be treated into the reaction tank 1 for surface treatment, performing oxidation reaction on the target object to be treated through ozone in the solution in the reaction tank 1, performing deoxidation treatment on the target object subjected to the oxidation reaction through hydrogen fluoride in the solution, and then taking out the treated target object to finish the treatment of one batch.
In some embodiments of the present invention, referring to fig. 1, 4 and 6, the following steps are further included after the step S4: s5: providing an inlet means and a discharge means, S6: communicating the liquid inlet device 3 and the liquid discharge device 4 with the reaction tank 1, respectively, and performing S7: a certain amount of solution is discharged through the liquid discharge device 4, and a certain amount of solution is replenished through the liquid inlet device 3.
In some embodiments of the present invention, the liquid inlet device 3 is disposed on the upper side of the reaction tank 1, the liquid inlet device 3 is used for introducing water and hydrogen fluoride into the reaction tank 1, and the liquid discharge device 4 is communicated with the bottom side surface of the reaction tank 1, so that when in use, liquid supplementing and discharging can be performed successively in the reaction tank 1 through the liquid inlet device 3 and the liquid discharge device 4, or simultaneously, liquid supplementing and discharging can be performed, and thus, the concentration of the hydrogen fluoride in the reaction tank 1 can be ensured.
In some embodiments of the present invention, referring to fig. 1 and 6, the step S4, after the target object to be processed is immersed in the reaction tank 1, includes the steps of: the temperature in the reaction tank 1 is controlled to be 25-30 ℃.
In some embodiments of the present invention, the temperature in the reaction tank 1 is controlled to be 27 ℃, and the temperature in the reaction tank 1 can be controlled to ensure the speed and effect of oxidation and deoxidation.
In some embodiments of the present invention, referring to fig. 1 and 6, in the step S6, the volume of the certain amount of solution in the certain amount of solution is discharged by the liquid discharge device 4 to be 0.5% to 10% of the volume of the solution in the reaction tank 1.
In some embodiments of the present invention, the volume of the certain amount of solution in the certain amount of solution discharged through the liquid discharge device 4 is 5% of the volume of the solution in the reaction tank 1, and the arrangement is such that the solution in the reaction tank 1 has little change and little influence on the reaction.
In a third embodiment of the present invention, a method for controlling a surface treatment apparatus includes controlling a concentration of the hydrofluoric acid solution in the step S2 to be 0.5%, controlling ozone generated by the ozone generating device 2 in the step S3 to enter the liquid circulation device 5 at a concentration of 150g/m3 and a flow rate of 5SLM, controlling a concentration of the ozone in the mixed solution to be 30ppm, controlling a temperature in the reaction tank 1 to be 25 ℃, and controlling a time for which a target object to be treated is immersed in the reaction tank 1 to be 60 seconds.
In a fourth embodiment of the present invention, a method for controlling a surface treatment apparatus includes controlling a concentration of the hydrofluoric acid solution in step S2 to be 1.5%, controlling ozone generated by the ozone generating device 2 in step S3 to enter the liquid circulation device 5 at a concentration of 400g/m3 and a flow rate of 50SLM, controlling a concentration of the ozone in the mixed solution to be 50ppm, controlling a temperature in the reaction tank 1 to be 25 ℃, and controlling a time for which a target object to be treated is immersed in the reaction tank 1 to be 5S.
In a fifth embodiment of the present invention, a method for controlling a surface treatment apparatus includes controlling a concentration of the hydrofluoric acid solution in step S2 to be 1%, controlling ozone generated by the ozone generating device 2 in step S3 to enter the liquid circulation device 5 at a concentration of 250g/m3 and a flow rate of 40SLM, controlling a concentration of the ozone in the mixed solution to be 40ppm, controlling a temperature in the reaction tank 1 to be 25 ℃, and controlling a time for which a target object to be treated is immersed in the reaction tank 1 to be 30S.
The electrical properties of the objects obtained by comparing the third, fourth and fifth examples were as follows:
in a sixth embodiment of the present invention, a method for controlling a surface treatment apparatus includes controlling a concentration of the hydrofluoric acid solution in step S2 to be 1%, controlling ozone generated by the ozone generating device 2 in step S3 to enter the liquid circulation device 5 at a concentration of 250g/m3 and a flow rate of 40SLM, controlling a concentration of the ozone in the mixed solution to be 40ppm, controlling a temperature in the reaction tank 1 to be 30 ℃, and controlling a time for which a target object to be treated is immersed in the reaction tank 1 to be 30S.
In a seventh embodiment of the present invention, a method for controlling a surface treatment apparatus includes controlling a concentration of the hydrofluoric acid solution in the step S2 to be 1%, controlling ozone generated by the ozone generating device 2 in the step S3 to enter the liquid circulation device 5 at a concentration of 250g/m3 and a flow rate of 40SLM, controlling a concentration of the ozone in the mixed solution to be 40ppm, controlling a temperature in the reaction tank 1 to be 27 ℃, and controlling a time for which a target object to be treated is immersed in the reaction tank 1 to be 30S.
The electrical properties of the object obtained by comparing the fifth, sixth and seventh examples were as follows:
although the embodiments of the present invention have been described in detail hereinabove, it is apparent to those skilled in the art that various modifications and variations can be made to these embodiments. However, it is to be understood that such modifications and variations are within the scope and spirit of the present invention as set forth in the following claims. Moreover, the invention as described herein is capable of other embodiments and of being practiced or of being carried out in various ways.
Claims (7)
1. A method of controlling a surface treatment apparatus, comprising the steps of:
s0: providing a reaction tank, a liquid circulating device and an ozone generating device;
s1: communicating the liquid circulation device with the reaction tank, and communicating the ozone generation device with the liquid circulation device;
s2: introducing a certain amount of hydrofluoric acid solution into the reaction tank;
s3: starting the ozone generating device to generate ozone, starting the liquid circulating device to drive the solution in the reaction tank to enter the liquid circulating device, mixing the solution entering the liquid circulating device with the ozone, and conveying the mixed solution back to the reaction tank;
s4: and immersing the target object to be treated in the reaction tank for surface treatment, and taking out.
2. The method of controlling a surface treatment apparatus according to claim 1, further comprising, after the step S4, the steps of:
s5: providing a liquid inlet device and a liquid discharge device;
s6: the liquid inlet device and the liquid discharge device are respectively communicated with the reaction tank;
s7: and discharging a certain amount of solution through the liquid discharging device, and supplementing a certain amount of solution through the liquid inlet device.
3. The method according to claim 1, wherein the concentration of the hydrofluoric acid solution in the step S2 is 0.5 to 1.5%.
4. The method of controlling a surface treatment apparatus according to claim 1, wherein the step of mixing the solution entering the liquid circulation device with the ozone in step S3 includes:
controlling the ozone generating device to generate ozone at 150-3And at a flow rate of 5-50SLM into the liquid circulation means.
5. The method of controlling a surface treatment apparatus according to claim 4, wherein in step S3, the concentration of ozone in the mixed solution is controlled to be 30-50 ppm.
6. The method for controlling a surface treatment apparatus according to claim 1, wherein the step S4, after immersing the object to be treated in the reaction tank, comprises the steps of: controlling the temperature in the reaction tank to be 25-30 ℃.
7. The method of controlling a surface treatment apparatus according to claim 2, wherein in step S7, the volume of the certain amount of solution in the certain amount of solution is discharged by the liquid discharge device to be 0.5% to 10% of the volume of the solution in the reaction tank.
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| JP2001326209A (en) * | 2000-05-16 | 2001-11-22 | Mitsubishi Materials Silicon Corp | Method for treating surface of silicon substrate |
| JP2002292379A (en) * | 2001-03-30 | 2002-10-08 | Nomura Micro Sci Co Ltd | Method and device for accelerated oxidation treatment |
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