CN113025994A - Furnace tube cleaning method - Google Patents
Furnace tube cleaning method Download PDFInfo
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- CN113025994A CN113025994A CN202110240477.7A CN202110240477A CN113025994A CN 113025994 A CN113025994 A CN 113025994A CN 202110240477 A CN202110240477 A CN 202110240477A CN 113025994 A CN113025994 A CN 113025994A
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- furnace tube
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- 238000000034 method Methods 0.000 title claims abstract description 60
- 238000004140 cleaning Methods 0.000 title claims abstract description 48
- 238000010926 purge Methods 0.000 claims abstract description 80
- 239000000428 dust Substances 0.000 claims abstract description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 64
- 229910052757 nitrogen Inorganic materials 0.000 claims description 32
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 23
- 238000005086 pumping Methods 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 5
- 229910021419 crystalline silicon Inorganic materials 0.000 description 11
- 238000000576 coating method Methods 0.000 description 10
- 230000000087 stabilizing effect Effects 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 7
- 229910052581 Si3N4 Inorganic materials 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000007888 film coating Substances 0.000 description 6
- 238000009501 film coating Methods 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000012459 cleaning agent Substances 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 206010027146 Melanoderma Diseases 0.000 description 2
- 241000519995 Stachys sylvatica Species 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4408—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber by purging residual gases from the reaction chamber or gas lines
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
- B08B9/027—Cleaning the internal surfaces; Removal of blockages
- B08B9/032—Cleaning the internal surfaces; Removal of blockages by the mechanical action of a moving fluid, e.g. by flushing
- B08B9/0321—Cleaning the internal surfaces; Removal of blockages by the mechanical action of a moving fluid, e.g. by flushing using pressurised, pulsating or purging fluid
- B08B9/0328—Cleaning the internal surfaces; Removal of blockages by the mechanical action of a moving fluid, e.g. by flushing using pressurised, pulsating or purging fluid by purging the pipe with a gas or a mixture of gas and liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
- B08B9/027—Cleaning the internal surfaces; Removal of blockages
- B08B9/032—Cleaning the internal surfaces; Removal of blockages by the mechanical action of a moving fluid, e.g. by flushing
- B08B9/035—Cleaning the internal surfaces; Removal of blockages by the mechanical action of a moving fluid, e.g. by flushing by suction
-
- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
-
- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention provides a furnace tube cleaning method, which comprises the following steps: sequentially purging and evacuating a furnace tube to complete one-time purging and evacuating operation, and repeating the purging and evacuating operation at least twice; (II) maintaining for a period of time after the pressure in the furnace tube is stabilized, then evacuating the furnace tube to complete one-time pressure-stabilizing evacuation operation, and repeating the pressure-stabilizing evacuation operation at least twice; and (III) cleaning, evacuating and inflating the furnace tube in sequence to finish the cleaning work of the furnace tube. The furnace tube cleaning method provided by the invention is adopted to clean the furnace tube after being used for many times, so that a good dust reduction effect can be obtained, the dust in the furnace tube can be effectively prevented from being adhered to the surface of a material in the working process of the furnace tube, and the probability of black spots and pockmarks on the surface of the material is reduced.
Description
Technical Field
The invention belongs to the technical field of furnace tube cleaning, and relates to a furnace tube cleaning method.
Background
PECVD, namely: plasma enhanced chemical vapor deposition. In PECVD, a gas containing atoms constituting a thin film is ionized by microwaves or radio frequencies to form a plasma locally, which is chemically very reactive and is easily reacted to deposit a desired thin film on a substrate. In order to allow chemical reactions to proceed at lower temperatures, the activity of the plasma is used to promote the reactions, and thus such CVD is called plasma-enhanced chemical vapor deposition.
In the production process of the solar photovoltaic cell, a layer of SiN is deposited on the surface of a graphite boat as a bearing silicon wafer in the process of operating a coating process in a PECVD furnace tubexA dielectric film. After the graphite boat is operated for a certain number of times to reach a certain saturation state, the silicon nitride powder falls off, so that the silicon nitride powder is slowly accumulated in the PECVD furnace tube in the film coating process. In addition, in the process of inserting the silicon wafer, the silicon wafer is fed into the PECVD furnace tube to operate a coating process under the condition that the process clamping point does not clamp the silicon wafer in place, and the silicon wafer which is not clamped in place also falls into the PECVD furnace tube. Over time, a large number of fragments and silicon nitride powder remain in the furnace after a number of process runs over a long period of time. In addition, during the process of processing an antireflection film of the crystalline silicon solar cell, part of powdery particles (silicon nitride powder) can be adsorbed on the surface of a semiconductor material for the solar cell, small white spots can be formed on part of the appearance after film coating, and black spots and pockmark states can be expressed in part of EL tests.
CN211725126U discloses an ash and slag mist collecting and purifying device suitable for a furnace blowing tube, which comprises a dust collecting box, wherein the dust collecting box is in a step shape with a low side and a high side, a box cover is buckled and connected on the correspondingly high side of the dust collecting box, a first baffle is vertically arranged in the dust collecting box, the dust collecting box is divided into a settling zone and a spraying zone by the first baffle, the dust collecting box contains water in the corresponding settling zone, an air guide pipe is arranged on one side of the dust collecting box corresponding to the settling zone, an air outlet is arranged on one side of the spraying zone corresponding to the side, a plurality of second baffles are vertically arranged in the corresponding spraying zone of the dust collecting box, the plurality of second baffles are sequentially staggered from top to bottom, the first baffle, the plurality of second baffles and the air outlet are sequentially arranged to form a plurality of bent air flow channels, and a plurality of rows of spraying heads are arranged at the positions of; the dust collection box is provided with a first sewage discharge port and a second sewage discharge port at the bottoms of the corresponding settling zone and the spraying zone respectively.
CN202230992U discloses an air inlet path device for DCE purging of a diffusion furnace tube, the air inlet path device is provided with a two-position three-way pneumatic valve, the inlet of the two-position three-way pneumatic valve is connected with a nitrogen source, the outlet of the two-position three-way pneumatic valve is provided with two air paths which are switched between a normally open end and a normally closed end, the two air paths are respectively connected with a one-way valve, and the other end of the one-way valve at the normally open end is connected with an exhaust device; the other end of the check valve at the normally closed end is connected to the air inlet of the DCE bubbling device, and the air outlet of the DCE bubbling device is communicated with the diffusion furnace tube through a third check valve.
CN106979718A discloses a method for cleaning a furnace tube of a heating furnace, comprising the following steps: (1) dissolving dirt: inputting a cleaning agent consisting of an organic solvent and an oil dispersing agent into a furnace tube, continuously and circularly cleaning the tube wall in the furnace tube, wherein the cleaning agent permeates, disperses and dissolves dirt, simultaneously monitoring the density of the cleaning agent, releasing part of solution when the saturated density of the organic solvent is reached, replenishing new organic solvent, repeatedly operating until the furnace tube is cleaned, and then exhausting the solution in the furnace tube; (2) washing: inputting a new cleaning agent into the furnace tube for washing to remove dirt remained in the furnace tube; (3) purging: and (4) carrying out nitrogen blasting purging on the furnace tube which is cleaned, and removing the residual cleaning agent in the furnace tube, namely finishing cleaning the furnace tube of the heating furnace.
Most fragments and silicon nitride powder are accumulated in the currently used PECVD furnace tube after long-time multiple coating, and part of powder particles (silicon nitride powder) can be adsorbed on the surface of a semiconductor material for a solar cell in the process of processing an antireflection film by a crystalline silicon solar cell. Therefore, when a solar cell is manufactured, the PECVD furnace tube is maintained by taking measures of chipping, cleaning enamel pores, cleaning tail rows and the like, and suspended dust exists in the maintained furnace tube and pipeline, so that the silicon wafer, the graphite boat and the like are polluted by dust when the process is directly operated without any treatment.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a furnace tube cleaning method, which is used for cleaning a furnace tube after being used for many times, so that a good dust reduction effect can be obtained, dust in the furnace tube can be effectively prevented from being adhered to the surface of a material in the working process of the furnace tube, and the probability of black spots and pockmarks on the surface of the material is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a furnace tube cleaning method, which comprises the following steps:
sequentially purging and evacuating a furnace tube to complete one-time purging and evacuating operation, and repeating the purging and evacuating operation at least twice;
(II) maintaining for a period of time after the pressure in the furnace tube is stabilized, then evacuating the furnace tube to complete one-time pressure-stabilizing evacuation operation, and repeating the pressure-stabilizing evacuation operation at least twice;
and (III) cleaning, evacuating and inflating the furnace tube in sequence to finish the cleaning work of the furnace tube.
As a preferred technical solution of the present invention, the furnace tube cleaning method further includes: pre-evacuating the furnace tube before step (I) is started, so that the interior of the furnace tube is in a vacuum state.
The furnace tube cleaning method provided by the invention is adopted to clean the furnace tube after being used for many times, so that a good dust reduction effect can be obtained, the dust in the furnace tube can be effectively prevented from being adhered to the surface of a material in the working process of the furnace tube, and the probability of black spots and pockmarks on the surface of the material is reduced.
Preferably, the pre-evacuation process comprises a slow evacuation and a main evacuation performed in sequence.
In a preferred embodiment of the present invention, the pumping time of the slow evacuation is 120 to 220s, for example, 120s, 130s, 140s, 150s, 160s, 170s, 180s, 190s, 200s, 210s, or 220s, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, after the slow evacuation is finished, the degree of vacuum in the furnace tube is less than or equal to 1520Pa, such as 500Pa, 600Pa, 700Pa, 800Pa, 900Pa, 1000Pa, 1100Pa, 1200Pa, 1300Pa, 1400Pa or 1500Pa, but the invention is not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a preferred embodiment of the present invention, the evacuation time of the main evacuation is 30 to 90s, and may be, for example, 30s, 35s, 40s, 45s, 50s, 55s, 60s, 65s, 70s, 75s, 80s, 85s, or 90s, but the evacuation time is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, after the main evacuation is finished, the degree of vacuum in the furnace tube is less than or equal to 30Pa, for example, 10Pa, 12Pa, 14Pa, 16Pa, 18Pa, 20Pa, 22Pa, 24Pa, 26Pa, 28Pa or 30Pa, but the degree of vacuum is not limited to the values listed, and other values not listed in the range of the values are also applicable.
In a preferred embodiment of the present invention, in step (i), the purge gas used in the purge process is nitrogen.
Preferably, the flow rate of the purge gas is 500 to 3500sccm, such as 500sccm, 1000sccm, 1500sccm, 2000sccm, 2500sccm, 3000sccm, 3500sccm, and more preferably 2000sccm, but the flow rate is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the temperature of the purging process is 420 to 600 ℃, for example, 420 ℃, 430 ℃, 440 ℃, 450 ℃, 460 ℃, 470 ℃, 480 ℃, 490 ℃, 500 ℃, 510 ℃, 520 ℃, 530 ℃, 540 ℃, 550 ℃, 560 ℃, 570 ℃, 580 ℃, 590 ℃ or 600 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the total time period of the purging is controlled to be 10-50 min, such as 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min or 50min, but not limited to the enumerated values, and other non-enumerated values in the numerical range are also applicable.
Preferably, the duration of each purge is 100-200 s, such as 100s, 110s, 120s, 130s, 140s, 150s, 160s, 170s, 180s, 190s, or 200s, but not limited to the recited values, and other unrecited values within the range of values are equally applicable.
In a preferred embodiment of the present invention, in step (i), the degree of vacuum in the furnace tube after evacuation is 30Pa or less, and may be, for example, 10Pa, 12Pa, 14Pa, 16Pa, 18Pa, 20Pa, 22Pa, 24Pa, 26Pa, 28Pa or 30Pa, but the degree is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
In a preferred embodiment of the present invention, in the step (ii), the pressure in the furnace tube is maintained for 100 to 280 seconds, for example, 100 seconds, 110 seconds, 120 seconds, 130 seconds, 140 seconds, 150 seconds, 160 seconds, 170 seconds, 180 seconds, 190 seconds, 200 seconds, 210 seconds, 220 seconds, 230 seconds, 240 seconds, 250 seconds, 260 seconds, 270 seconds, or 280 seconds, but the present invention is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the furnace tube is evacuated to a vacuum of 30Pa or less, which may be, for example, 10Pa, 12Pa, 14Pa, 16Pa, 18Pa, 20Pa, 22Pa, 24Pa, 26Pa, 28Pa or 30Pa, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
As a preferred embodiment of the present invention, in step (iii), the cleaning process includes: and introducing nitrogen into the furnace tube, and completely emptying residual gas and dust in the furnace tube.
Preferably, the degree of vacuum in the furnace tube after evacuation is less than or equal to 30Pa, and may be, for example, 10Pa, 12Pa, 14Pa, 16Pa, 18Pa, 20Pa, 22Pa, 24Pa, 26Pa, 28Pa or 30Pa, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the inflation process comprises: and introducing nitrogen into the furnace tube to ensure that the pressure in the furnace tube is consistent with the external pressure.
As a preferred technical solution of the present invention, the furnace tube cleaning method further includes: and (3) completely circulating at least twice according to the sequence of the step (I), the step (II) and the step (III).
As a preferred technical scheme of the invention, the furnace tube is a PECVD furnace tube.
Compared with the prior art, the invention has the beneficial effects that:
the furnace tube cleaning method provided by the invention is adopted to clean the furnace tube after being used for many times, so that a good dust reduction effect can be obtained, the dust in the furnace tube can be effectively prevented from being adhered to the surface of a material in the working process of the furnace tube, and the probability of black spots and pockmarks on the surface of the material is reduced.
Drawings
Fig. 1 is a schematic structural diagram of a furnace tube cleaning method provided in embodiment 1 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
Example 1
The present embodiment provides a furnace tube cleaning method, as shown in fig. 1, including the following steps:
(1) performing slow evacuation and main evacuation in sequence in the furnace tube, wherein the air evacuation time of the slow evacuation is 120s, and after the slow evacuation is finished, the vacuum degree in the furnace tube is 1520 Pa; the evacuation time of the main evacuation is 30s, and after the main evacuation is finished, the vacuum degree in the furnace tube is 30 Pa;
(2) purging the furnace tube by adopting nitrogen, wherein the flow of the nitrogen is 500sccm, and the purging temperature is 420 ℃; after purging is finished, evacuating the furnace tube, and pumping the vacuum degree in the furnace tube to 30Pa to finish one-time purging and evacuating operation; then repeating the purging and evacuating operations for 3 times, wherein the time of each purging is controlled to be 200s, and the total purging time in the whole purging and evacuating process is controlled to be 10 min;
(3) after the circulation of the purging and evacuating operations is finished, maintaining the pressure in the furnace tube for 100s after the pressure in the furnace tube is stabilized, and then pumping the vacuum degree in the furnace tube to 30Pa to finish one-time pressure-stabilizing and evacuating operation; then repeating the pressure-stabilizing evacuation operation for 2 times;
(4) after the pressure stabilizing evacuation operation cycle is finished, nitrogen is introduced into the furnace tube, residual gas and dust in the furnace tube are completely evacuated, then the vacuum degree in the furnace tube is pumped to 30Pa, and finally nitrogen is introduced into the furnace tube, so that the pressure in the furnace tube is kept consistent with the external pressure.
The cleaned PECVD furnace tube is adopted to coat the surface of the crystalline silicon solar cell, the proportion of black spots and the proportion of pockmarks on the coated surface are observed and calculated, and the dust pollution degree of the coating is evaluated, and the result is shown in Table 1.
Example 2
The present embodiment provides a furnace tube cleaning method, as shown in fig. 1, including the following steps:
(1) carrying out slow evacuation and main evacuation in sequence in the furnace tube, wherein the air evacuation time of the slow evacuation is 140s, and the vacuum degree in the furnace tube is 1000Pa after the slow evacuation is finished; the evacuation time of the main evacuation is 45s, and after the main evacuation is finished, the vacuum degree in the furnace tube is 23 Pa;
(2) purging the furnace tube by adopting nitrogen, wherein the flow of the nitrogen is 1000sccm, and the purging temperature is 450 ℃; after purging is finished, evacuating the furnace tube, and pumping the vacuum degree in the furnace tube to 23Pa to finish one-time purging and evacuating operation; then repeating the purging and evacuating operations for 6 times, wherein the time of each purging is controlled to be 100s, and the total purging time in the whole purging and evacuating process is controlled to be 10 min;
(3) after the circulation of the purging and evacuating operation is finished, maintaining the pressure in the furnace tube for 140s after the pressure in the furnace tube is stabilized, and then pumping the vacuum degree in the furnace tube to 23Pa to finish the primary pressure stabilizing and evacuating operation; then repeating the pressure-stabilizing evacuation operation at least twice;
(4) after the pressure stabilizing evacuation operation cycle is finished, nitrogen is introduced into the furnace tube, residual gas and dust in the furnace tube are completely evacuated, then the vacuum degree in the furnace tube is pumped to 23Pa, and finally nitrogen is introduced into the furnace tube, so that the pressure in the furnace tube is kept consistent with the external pressure.
The cleaned PECVD furnace tube is adopted to coat the surface of the crystalline silicon solar cell, the proportion of black spots and the proportion of pockmarks on the coated surface are observed and calculated, and the dust pollution degree of the coating is evaluated, and the result is shown in Table 1.
Example 3
The present embodiment provides a furnace tube cleaning method, as shown in fig. 1, including the following steps:
(1) performing slow evacuation and main evacuation in sequence in the furnace tube, wherein the air evacuation time of the slow evacuation is 160s, and the vacuum degree in the furnace tube is 800Pa after the slow evacuation is finished; the evacuation time of the main evacuation is 55s, and after the main evacuation is finished, the vacuum degree in the furnace tube is 20 Pa;
(2) purging the furnace tube by adopting nitrogen, wherein the flow of the nitrogen is 1600sccm, and the purging temperature is 500 ℃; after purging is finished, evacuating the furnace tube, and pumping the vacuum degree in the furnace tube to 20Pa to finish one-time purging and evacuating operation; then repeating the purging and evacuating operations for 6 times, wherein the time of each purging is controlled to be 120s, and the total purging time in the whole purging and evacuating process is controlled to be 12 min;
(3) after the circulation of the purging and evacuating operation is finished, maintaining the pressure in the furnace tube for 180s after the pressure in the furnace tube is stabilized, and then pumping the vacuum degree in the furnace tube to 20Pa to finish the primary pressure stabilizing and evacuating operation; then repeating the pressure stabilizing and pumping operation for 5 times;
(4) after the pressure stabilizing evacuation operation cycle is finished, nitrogen is introduced into the furnace tube, residual gas and dust in the furnace tube are completely evacuated, then the vacuum degree in the furnace tube is pumped to 20Pa, and finally nitrogen is introduced into the furnace tube, so that the pressure in the furnace tube is kept consistent with the external pressure.
The cleaned PECVD furnace tube is adopted to coat the surface of the crystalline silicon solar cell, the proportion of black spots and the proportion of pockmarks on the coated surface are observed and calculated, and the dust pollution degree of the coating is evaluated, and the result is shown in Table 1.
Example 4
The present embodiment provides a furnace tube cleaning method, as shown in fig. 1, including the following steps:
(1) performing slow evacuation and main evacuation in sequence in the furnace tube, wherein the air evacuation time of the slow evacuation is 180s, and the vacuum degree in the furnace tube is 700Pa after the slow evacuation is finished; the evacuation time of the main evacuation is 70s, and after the main evacuation is finished, the vacuum degree in the furnace tube is 16 Pa;
(2) purging the furnace tube by adopting nitrogen, wherein the flow rate of the nitrogen is 2300sccm, and the purging temperature is 530 ℃; after purging is finished, evacuating the furnace tube, and pumping the vacuum degree in the furnace tube to 16Pa to finish one-time purging and evacuating operation; then repeating the purging and evacuating operations for 10 times, wherein the time of each purging is controlled to be 150s, and the total purging time in the whole purging and evacuating process is controlled to be 25 min;
(3) after the circulation of the purging and evacuating operations is finished, maintaining the pressure in the furnace tube for 220s after the pressure in the furnace tube is stabilized, and then pumping the vacuum degree in the furnace tube to 16Pa to finish one-time pressure-stabilizing and evacuating operation; then repeating the operation of pressure stabilization and evacuation for 6 times;
(4) after the pressure stabilizing evacuation operation cycle is finished, nitrogen is introduced into the furnace tube, residual gas and dust in the furnace tube are completely evacuated, then the vacuum degree in the furnace tube is pumped to 16Pa, and finally nitrogen is introduced into the furnace tube, so that the pressure in the furnace tube is kept consistent with the external pressure.
And (4) repeating the steps (1) to (4) once again.
The cleaned PECVD furnace tube is adopted to coat the surface of the crystalline silicon solar cell, the proportion of black spots and the proportion of pockmarks on the coated surface are observed and calculated, and the dust pollution degree of the coating is evaluated, and the result is shown in Table 1.
Example 5
The present embodiment provides a furnace tube cleaning method, as shown in fig. 1, including the following steps:
(1) performing slow evacuation and main evacuation in sequence in the furnace tube, wherein the air evacuation time of the slow evacuation is 200s, and the vacuum degree in the furnace tube is 600Pa after the slow evacuation is finished; the evacuation time of the main evacuation is 80s, and after the main evacuation is finished, the vacuum degree in the furnace tube is 13 Pa;
(2) purging the furnace tube by adopting nitrogen, wherein the flow of the nitrogen is 3000sccm, and the purging temperature is 560 ℃; after purging is finished, evacuating the furnace tube, and pumping the vacuum degree in the furnace tube to 13Pa to finish one-time purging and evacuating operation; then repeating the purging and evacuating operations for 8 times, wherein the time of each purging is controlled to be 180s, and the total purging time in the whole purging and evacuating process is controlled to be 24 min;
(3) after the circulation of the purging and evacuating operation is finished, maintaining the pressure in the furnace tube for 250s after the pressure in the furnace tube is stabilized, and then pumping the vacuum degree in the furnace tube to 13Pa to finish the primary pressure stabilizing and evacuating operation; then repeating the operation of pressure stabilization and evacuation for 7 times;
(4) after the pressure stabilizing evacuation operation cycle is finished, nitrogen is introduced into the furnace tube, residual gas and dust in the furnace tube are completely evacuated, then the vacuum degree in the furnace tube is pumped to 13Pa, and finally nitrogen is introduced into the furnace tube, so that the pressure in the furnace tube is kept consistent with the external pressure.
And (4) repeating the steps (1) to (4) once again.
The cleaned PECVD furnace tube is adopted to coat the surface of the crystalline silicon solar cell, the proportion of black spots and the proportion of pockmarks on the coated surface are observed and calculated, and the dust pollution degree of the coating is evaluated, and the result is shown in Table 1.
Example 6
The present embodiment provides a furnace tube cleaning method, as shown in fig. 1, including the following steps:
(1) carrying out slow evacuation and main evacuation in sequence in the furnace tube, wherein the air evacuation time of the slow evacuation is 220s, and the vacuum degree in the furnace tube is 500Pa after the slow evacuation is finished; the evacuation time of the main evacuation is 90s, and after the main evacuation is finished, the vacuum degree in the furnace tube is 10 Pa;
(2) purging the furnace tube by adopting nitrogen, wherein the flow of the nitrogen is 3500sccm, and the purging temperature is 600 ℃; after purging is finished, evacuating the furnace tube, and pumping the vacuum degree in the furnace tube to 10Pa to finish one-time purging and evacuating operation; then repeating the purging and evacuating operations for 15 times, wherein the time of each purging is controlled to be 200s, and the total purging time in the whole purging and evacuating process is controlled to be 50 min;
(3) after the circulation of the purging and evacuating operation is finished, maintaining the pressure in the furnace tube for 280s, and then pumping the vacuum degree in the furnace tube to 10Pa to finish one-time pressure-stabilizing and evacuating operation; then repeating the voltage stabilization pumping-out operation for 10 times;
(4) after the pressure stabilizing evacuation operation cycle is finished, nitrogen is introduced into the furnace tube, residual gas and dust in the furnace tube are completely evacuated, then the vacuum degree in the furnace tube is pumped to 10Pa, and finally nitrogen is introduced into the furnace tube, so that the pressure in the furnace tube is kept consistent with the external pressure.
And (4) repeating the steps (1) to (4) once again.
The cleaned PECVD furnace tube is adopted to coat the surface of the crystalline silicon solar cell, the proportion of black spots and the proportion of pockmarks on the coated surface are observed and calculated, and the dust pollution degree of the coating is evaluated, and the result is shown in Table 1.
Comparative example 1
The PECVD furnace tube is observed after long-time and multiple times of film coating, and more silicon nitride fragments are remained and accumulated in the tube.
The PECVD furnace tube without any cleaning treatment is adopted to carry out film coating on the surface of the crystalline silicon solar cell, the black spot proportion and the pockmark proportion of the film coating surface are observed and calculated, and the dust pollution degree of the film coating is evaluated, and the result is shown in table 1.
Comparative example 2
On the basis of the comparative example 1, manual operations such as chipping, cleaning enamel pores, cleaning tail rows and the like are performed in the PECVD furnace tube, but the purging process of the PECVD furnace tube is not used for purging.
The cleaned PECVD furnace tube is adopted to coat the surface of the crystalline silicon solar cell, the proportion of black spots and the proportion of pockmarks on the coated surface are observed and calculated, and the dust pollution degree of the coating is evaluated, and the result is shown in Table 1.
TABLE 1
The comparison of the appearances of the coated crystalline silicon solar cells shows that the integral consistency of small white spots on the film surface is reduced after the cleaning method provided by the invention is adopted. As can be seen from the data in Table 1, the black spot ratio and the pockmark ratio were decreased more advantageously when the furnace tube without any cleaning treatment (comparative example 1) was used than when the furnace tubes were treated by the cleaning method provided by the present invention (examples 1-6); and the first furnace can reach 100% dust pollution after manual maintenance.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A furnace tube cleaning method is characterized by comprising the following steps:
sequentially purging and evacuating a furnace tube to complete one-time purging and evacuating operation, and repeating the purging and evacuating operation at least twice;
(II) maintaining for a period of time after the pressure in the furnace tube is stabilized, then evacuating the furnace tube to complete one-time pressure-stabilizing evacuation operation, and repeating the pressure-stabilizing evacuation operation at least twice;
and (III) cleaning, evacuating and inflating the furnace tube in sequence to finish the cleaning work of the furnace tube.
2. The furnace tube cleaning method of claim 1, further comprising: pre-evacuating the furnace tube before the step (I) is started, so that the interior of the furnace tube is in a vacuum state;
preferably, the pre-evacuation process comprises a slow evacuation and a main evacuation performed in sequence.
3. The furnace tube cleaning method of claim 2, wherein the pumping time of the slow pumping is 120-220 s;
preferably, after the slow evacuation is finished, the vacuum degree in the furnace pipe is less than or equal to 1520 Pa.
4. The furnace tube cleaning method according to claim 2 or 3, wherein the evacuation time of the main evacuation is 30-90 s;
preferably, after the main evacuation is finished, the vacuum degree in the furnace tube is less than or equal to 30 Pa.
5. The furnace tube cleaning method according to any of claims 1-4, wherein in step (I), the purge gas used in the purge process is nitrogen;
preferably, the flow rate of the purge gas is 500-3500 sccm, and more preferably 2000 sccm;
preferably, the temperature of the purging process is 420-600 ℃;
preferably, the total time of purging is controlled to be 10-50 min;
preferably, the time length of each purging is 100-200 s.
6. The furnace tube cleaning method according to any one of claims 1 to 5, wherein in step (I), the degree of vacuum in the furnace tube after evacuation is 30Pa or less.
7. The furnace tube cleaning method according to any one of claims 1-6, wherein in the step (II), the pressure in the furnace tube is maintained for 100-280 s;
preferably, the furnace tube is evacuated to the vacuum degree of less than or equal to 30 Pa.
8. The furnace tube cleaning method according to any of claims 1-7, wherein in step (III), the cleaning process comprises: introducing nitrogen into the furnace tube, and completely emptying residual gas and dust in the furnace tube;
preferably, the vacuum degree in the furnace tube after being pumped out is less than or equal to 30 Pa;
preferably, the inflation process comprises: and introducing nitrogen into the furnace tube to ensure that the pressure in the furnace tube is consistent with the external pressure.
9. The furnace tube cleaning method according to any one of claims 1-8, further comprising: and (3) completely circulating at least twice according to the sequence of the step (I), the step (II) and the step (III).
10. The method of any one of claims 1 to 9, wherein the furnace is a PECVD furnace.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113481487A (en) * | 2021-07-06 | 2021-10-08 | 横店集团东磁股份有限公司 | Solar cell and back surface PECVD method and application thereof |
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