CN109107974B - Cleaning method of quartz device for solar cell preparation - Google Patents

Cleaning method of quartz device for solar cell preparation Download PDF

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CN109107974B
CN109107974B CN201810805202.1A CN201810805202A CN109107974B CN 109107974 B CN109107974 B CN 109107974B CN 201810805202 A CN201810805202 A CN 201810805202A CN 109107974 B CN109107974 B CN 109107974B
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cleaning
quartz device
quartz
solar cell
ozone water
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CN109107974A (en
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许成德
陈健生
李鑫
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Qixian Dongci New Energy Co ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/04—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by a combination of operations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B2203/00—Details of cleaning machines or methods involving the use or presence of liquid or steam
    • B08B2203/005—Details of cleaning machines or methods involving the use or presence of liquid or steam the liquid being ozonated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B2203/00—Details of cleaning machines or methods involving the use or presence of liquid or steam
    • B08B2203/007—Heating the liquid

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cleaning By Liquid Or Steam (AREA)

Abstract

The invention belongs to the technical field of solar cells. The invention discloses a method for cleaning a quartz device for solar cell preparation, which comprises the steps of cleaning a cleaning tank by acid, cleaning a high-temperature water washing tank by water, cleaning the normal-temperature water washing tank by water, drying and the like, wherein the acid cleaning is carried out by adopting mixed liquid medicine of hydrofluoric acid and ozone water, and the water cleaning is carried out by adopting ozone water. The invention is not only suitable for quartz devices in a diffusion process, but also suitable for cleaning the quartz devices in a film coating process; the invention can reduce the usage amount of hydrofluoric acid, hydrochloric acid and ozone water, and greatly reduce the time of the whole cleaning process; the invention can effectively clean the quartz device, reduce the pollution proportion and improve the efficiency.

Description

Cleaning method of quartz device for solar cell preparation
Technical Field
The invention relates to the technical field of solar cells, in particular to a method for cleaning a quartz device for preparing a solar cell.
Background
The diffusion process is a process for forming a P-N junction in the production of a crystalline silicon solar cell. The silicon wafer diffusion process is a process of generating elemental phosphorus by chemical reaction of diffusion source gas and a silicon wafer at high temperature and depositing the elemental phosphorus on the surface of a P-type crystal silicon, and the chemical reaction formula is as follows:
Figure BDA0001738022460000011
2P2O5+5Si＝＝5SiO2+4P↓，
as can be seen from the above reaction formula, POCl3When thermally decomposed, if there is no external oxygen (O)2) Generated PCl is not sufficient to participate in decomposition5Is not easy to decompose, has corrosion effect on silicon and damages the surface state of the silicon wafer. But in the presence of foreign O2In the presence of PCl5Will be further decomposed into P2O5And chlorine (Cl) is discharged2) The reaction formula is as follows:
Figure BDA0001738022460000012
generated P2O5Further reacts with silicon to form SiO2And a phosphorus atom.
During diffusion, the silicon wafer is firstly inserted into a quartz boat, and then the quartz boat and the silicon wafer are placed into a diffusion quartz tube for diffusion process. After the diffusion is finished, the silicon wafers are taken out of the quartz boat, and then new silicon wafers are inserted for the next batch of diffusion, so that the quartz devices are reused in the production process. However, a layer of white powder is deposited on the surface of the quartz device after long-term use, and the white powder is composed of a mixture of phosphorus pentoxide, metaphosphoric acid, orthophosphoric acid, phosphorus pentachloride, dust, silicon chip scraps and the like. When exposed to air, quartz devices chemically react with moisture in the air, and the following reaction equation:
P2O5+H22HPO (low temperature)3，
P2O5+3H2O (high temperature) ═ 2H3PO4，
PCl5+H2O (small amount) ═ POCl3+2HCl，
PCl5+4H2O (excess) ═ H3PO4+5HCl，
The quartz device includes: quartz tube, quartz boat, waste discharge tube, tail gas cylinder, etc., and will not be explained in more detail later.
When a large amount of mixture is generated on the surface of the quartz device, and after each diffusion process, a certain amount of diffused dust and particles remain on the surface of the quartz device, and the surface of the quartz device is affected by contacting with a silicon wafer, for example: the card slot is printed with black spots and the like, and even reduces the efficiency of the battery piece when serious. Therefore, the quartz boat needs to be cleaned regularly.
The existing cleaning method of the quartz device comprises the steps of firstly carrying out acid cleaning by adopting mixed acid of hydrofluoric acid and hydrochloric acid, then carrying out water cleaning by adopting a pure water overflow mode, and finally drying; the cleaning process flow of the quartz device has the following problems that the original pickling tank is designed to be uncovered for simple operation, hydrofluoric acid and hydrochloric acid volatilize in the pickling process of the quartz device to cause the workshop to smell bad sour, the concentration of the pickling tank is always in the process of reduction due to continuous volatilization of the hydrofluoric acid and the hydrochloric acid, the pickling and water washing time is too long, chemicals of the hydrofluoric acid and the hydrochloric acid are used too much, the cleaned quartz device is not cleaned completely, and the cleaned quartz device has acid residues to cause EL pollution of a battery piece.
Disclosure of Invention
In order to solve the problems, the invention provides a method for cleaning a quartz device for solar cell preparation, which can reduce the use of chemicals and greatly save water resources and cleaning time under the condition of ensuring that the cleaning quality is not reduced.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for cleaning a quartz device for solar cell preparation comprises the following steps:
a) adding mixed liquid medicine of hydrofluoric acid and ozone water into the cleaning tank, heating, and placing the quartz device into the cleaning tank for sealing, soaking and pickling;
b) adding ozone water into a high-temperature rinsing bath, heating, and soaking and cleaning the quartz device soaked and pickled in the step a) in the high-temperature rinsing bath;
c) adding ozone water into the normal-temperature water washing tank, and soaking and washing the quartz device soaked and washed in the step b) in the normal-temperature water washing tank at normal temperature;
d) repeating the step c) until the pH value of the normal-temperature rinsing bath is neutral, and finishing rinsing;
e) and taking out the quartz device after the water washing is finished, and drying to finish the cleaning process of the quartz device.
Preferably, the ozone content in the ozone water is 10-30 ppm.
Preferably, in the mixed chemical liquid of hydrofluoric acid and ozone water, the volume ratio of hydrofluoric acid to ozone water is (1-2): (15-20).
Preferably, in the step a), the temperature is controlled to be 60-90 ℃ during soaking and pickling, and 40KHz ultrasonic waves and bubbling are used for assisting pickling.
Preferably, in the step a), the soaking and pickling time is 15-40 minutes.
Preferably, in the step b), the temperature is controlled to be 60-90 ℃ during soaking and cleaning, and 40KHz ultrasonic waves and bubbling are used for assisting cleaning.
Preferably, in the step b), the volume of the ozone water is kept to be 200-250L, and the soaking and cleaning time is 10-30 minutes.
Preferably, in step c), bubbling assisted cleaning is used for immersion cleaning.
Preferably, in the step c), the volume of the ozone water is kept to be 200-250L, and the soaking and cleaning time is 10-30 minutes.
Preferably, in step e), the removed quartz device is dried using nitrogen or compressed air.
In the step a), in order to accelerate the pickling rate and enhance the cleaning effect, the bottom of the cleaning tank is heated, so that the quartz device is pickled at a high temperature; hydrofluoric acid is volatile acid, ozone in ozone water can be decomposed into oxygen to be volatilized, particularly in a high-temperature bubbling opening state, so that the top of the cleaning tank is covered with a cover, the cover is sealed, effective sealing can be guaranteed in a high-temperature state, and volatilization of hydrofluoric acid and decomposition of ozone are prevented.
In the step b), in order to make acid on the surface of the quartz device quickly and effectively separate from the quartz device, ozone water is adopted for cleaning at a high temperature, and hydrofluoric acid is quickly dissolved in ozone water at the high temperature, so that hydrofluoric acid components on the surface of the quartz device are effectively removed.
The ozone water has a very strong oxidizing power and a very strong oxidizing property, and the oxidation-reduction potential of the ozone water is higher than that of sulfuric acid, hydrofluoric acid and hydrogen peroxide. Therefore, the efficiency of removing organic matter and metal using ozone water is better than that of the conventional method.
Therefore, the invention has the following beneficial effects:
(1) the invention is not only suitable for quartz devices in a diffusion process, but also suitable for cleaning the quartz devices in a film coating process;
(2) the invention can reduce the usage amount of hydrofluoric acid, hydrochloric acid and ozone water, and greatly reduce the time of the whole cleaning process;
(3) the invention can effectively clean the quartz device, reduce the pollution proportion and improve the efficiency.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. 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.
In the present invention, all the equipments and materials are commercially available or commonly used in the industry, and the methods in the following examples are conventional in the art unless otherwise specified.
Hydrofluoric acid and hydrochloric acid used in the following examples and comparative examples were commercially available raw materials, wherein the concentration of hydrofluoric acid was 49 wt% and the concentration of hydrochloric acid was 37 wt%.
Example 1
A method for cleaning a quartz device for solar cell preparation comprises the following steps:
a) adding 10L of hydrofluoric acid and 150L of ozone water into a cleaning tank to obtain mixed liquid medicine, heating to 60 ℃, putting the quartz device into the cleaning tank, sealing, soaking and pickling for 15 minutes, and using 40KHz ultrasonic waves and bubbling to assist pickling;
b) adding ozone water into a high-temperature water washing tank, keeping the volume of the ozone water at 230L, heating to 60 ℃, soaking and cleaning the quartz device soaked and pickled in the step a) in the high-temperature water washing tank for 10 minutes, and using 40KHz ultrasonic waves and bubbling for auxiliary cleaning;
c) adding ozone water into a normal-temperature water washing tank, keeping the volume of the ozone water at 230L, soaking and washing the quartz device soaked and washed in the step b) in the normal-temperature water washing tank for 10 minutes at normal temperature, and using bubbling to assist in washing;
d) repeating the step c) once until the pH value of the normal-temperature water washing tank is 7, and finishing the water washing;
e) and taking out the quartz device after the water washing is finished, and drying the taken out quartz device by adopting nitrogen to finish the cleaning process of the quartz device.
Wherein, the ozone content in the ozone water in the process is 10 ppm.
Example 2
A method for cleaning a quartz device for solar cell preparation comprises the following steps:
a) adding 20L of hydrofluoric acid and 200L of ozone water into a cleaning tank to obtain mixed liquid medicine, heating to 90 ℃, putting the quartz device into the cleaning tank, sealing, soaking and pickling for 30 minutes, and using 40KHz ultrasonic waves and bubbling to assist pickling;
b) adding ozone water into a high-temperature water washing tank, keeping the volume of the ozone water at 250L, heating to 90 ℃, soaking and cleaning the quartz device soaked and pickled in the step a) in the high-temperature water washing tank for 30 minutes, and using 40KHz ultrasonic waves and bubbling for auxiliary cleaning;
c) adding ozone water into a normal-temperature water washing tank, keeping the volume of the ozone water at 250L, soaking and washing the quartz device soaked and washed in the step b) in the normal-temperature water washing tank for 30 minutes at normal temperature, and using bubbling to assist in washing;
d) repeating the step c) once until the pH value of the normal-temperature water washing tank is 7, and finishing the water washing;
e) and taking out the quartz device after the water washing is finished, and drying the taken out quartz device by adopting compressed air to finish the cleaning process of the quartz device.
Wherein, the ozone content in the ozone water in the process is 30 ppm.
Example 3
A method for cleaning a quartz device for solar cell preparation comprises the following steps:
a) adding 20L of hydrofluoric acid and 160L of ozone water into a cleaning tank to obtain mixed liquid medicine, heating to 70 ℃, putting the quartz device into the cleaning tank, sealing, soaking and pickling for 40 minutes, and using 40KHz ultrasonic waves and bubbling to assist in pickling;
b) adding ozone water into a high-temperature water washing tank, keeping the volume of the ozone water at 200L, heating to 80 ℃, soaking and cleaning the quartz device soaked and pickled in the step a) in the high-temperature water washing tank for 15 minutes, and using 40KHz ultrasonic waves and bubbling for auxiliary cleaning;
c) adding ozone water into a normal-temperature water washing tank, keeping the volume of the ozone water at 200L, soaking and washing the quartz device soaked and washed in the step b) in the normal-temperature water washing tank for 15 minutes at normal temperature, and using bubbling to assist in washing;
d) repeating the step c) once until the pH value of the normal-temperature water washing tank is 7, and finishing the water washing;
e) and taking out the quartz device after the water washing is finished, and drying the taken out quartz device by adopting nitrogen to finish the cleaning process of the quartz device.
Wherein, the ozone content in the ozone water in the process is 20 ppm.
Example 4
A method for cleaning a quartz device for solar cell preparation comprises the following steps:
a) adding 16L of hydrofluoric acid and 160L of ozone water into a cleaning tank, mixing to obtain a mixed liquid medicine, heating to 80 ℃, putting the quartz device into the cleaning tank, sealing, soaking and pickling for 40 minutes, and using 40KHz ultrasonic waves and bubbling to assist in pickling;
b) adding ozone water into a high-temperature water washing tank, keeping the volume of the ozone water at 200L, heating to 80 ℃, soaking and cleaning the quartz device soaked and pickled in the step a) in the high-temperature water washing tank for 15 minutes, and using 40KHz ultrasonic waves and bubbling for auxiliary cleaning;
c) adding ozone water into a normal-temperature water washing tank, keeping the volume of the ozone water at 200L, soaking and washing the quartz device soaked and washed in the step b) in the normal-temperature water washing tank for 15 minutes at normal temperature, and using bubbling to assist in washing;
d) repeating the step c) once until the pH value of the normal-temperature water washing tank is 7, and finishing the water washing;
e) and taking out the quartz device after the water washing is finished, and drying the taken out quartz device by adopting compressed air to finish the cleaning process of the quartz device.
Wherein, the ozone content in the ozone water in the process is 20 ppm.
Example 5
A method for cleaning a quartz device for solar cell preparation comprises the following steps:
a) adding 12L of hydrofluoric acid and 160L of ozone water into a cleaning tank, mixing to obtain a mixed liquid medicine, heating to 90 ℃, putting the quartz device into the cleaning tank, sealing, soaking and pickling for 40 minutes, and using 40KHz ultrasonic waves and bubbling to assist in pickling;
b) adding ozone water into a high-temperature water washing tank, keeping the volume of the ozone water at 200L, heating to 80 ℃, soaking and cleaning the quartz device soaked and pickled in the step a) in the high-temperature water washing tank for 15 minutes, and using 40KHz ultrasonic waves and bubbling for auxiliary cleaning;
c) adding ozone water into a normal-temperature water washing tank, keeping the volume of the ozone water at 200L, soaking and washing the quartz device soaked and washed in the step b) in the normal-temperature water washing tank for 15 minutes at normal temperature, and using bubbling to assist in washing;
d) repeating the step c) once until the pH value of the normal-temperature water washing tank is 7, and finishing the water washing;
e) and taking out the quartz device after the water washing is finished, and drying the taken out quartz device by adopting nitrogen to finish the cleaning process of the quartz device.
Wherein, the ozone content in the ozone water in the process is 20 ppm.
Comparative example
1) Adding a mixed liquid medicine with the proportion of 32 liters of hydrofluoric acid, 16 liters of hydrochloric acid and 160 liters of water into a cleaning tank, soaking and pickling the quartz device for 90 minutes at normal temperature, using ultrasonic waves with the frequency of 40KHz and adding bubbling to assist in cleaning, wherein the cleaning tank is in an open state;
2) taking out the quartz device which is well pickled, putting the quartz device in a 1-tank water washing process to use an overflow mode, using 500 liters of pure water, cleaning for 40min, using ultrasonic waves with the frequency of 40KHz, and adding bubbles to assist in cleaning;
3) placing the quartz device in a water washing 2 tank using an overflow mode, using 500 liters of pure water, cleaning for 40min, using ultrasonic waves with the frequency of 40KHz, and adding bubbles to assist in cleaning;
4) placing the quartz device in a 3-tank water washing tank to use an overflow mode, using 500 liters of pure water, washing for 40min, using ultrasonic waves with the frequency of 40KHz, and adding bubbles to assist in washing;
5) testing the water tank by using pH test paper until the water tank is neutral, and taking the pH test paper as a judgment standard;
6) and (4) after the water washing is finished, taking out the quartz boat, and blowing by using nitrogen or compressed air until the quartz boat is dried to finish the quartz boat washing process.
And (3) testing the cleaning efficiency and the effect:
selecting six groups of quartz boats to be cleaned, respectively cleaning by the methods in the embodiments 1-5 and the comparative example, and simultaneously recording data such as consumed hydrofluoric acid and ozone water; and then 6000 pieces of P-type 156.75 multiplied by 156.75 monocrystalline silicon pieces are selected, a conventional alkali texturing process is carried out, the textured surface is manufactured and then is uniformly divided into 6 groups by using a card-dealing type, the quartz boats cleaned in the above mode are respectively used for diffusion treatment, and data such as efficiency, pollution and the like are tracked.
And (3) testing results:
examples 1-5 and comparative examples chemical consumption are given in table 1 below:
TABLE 1
Figure BDA0001738022460000061
The quartz boats obtained after cleaning in examples 1 to 5 and comparative example were used for the following 6 groups of wafers after texturing, and data of slot prints, black dot number, efficiency, pollution and the like after diffusion tracking are shown in the following table 2:
TABLE 2
Figure BDA0001738022460000062
Combining the comparative examples with the comparative groups, it can be seen that:
1. the consumption of chemicals for cleaning the quartz boat by using the novel method for cleaning the quartz device is obviously less than that of the original method for cleaning the quartz device;
2. the time for cleaning the quartz boat by using the novel method for cleaning the quartz device is obviously at least 90 minutes less than that of the original method for cleaning the quartz device;
3. the diffusion of the quartz boat cleaned by the novel quartz device cleaning method is obviously less by 0.2-0.3% than that of the quartz boat cleaned by the original quartz device cleaning method;
4. the diffusion of the quartz boat cleaned by the novel quartz device cleaning method is obviously 0.3-0.7% less than that of the diffusion clamping groove printing and black spot of the quartz boat cleaned by the original quartz device cleaning method;
5. the diffusion efficiency of the quartz boat cleaned by the novel quartz device cleaning method is obviously 0.02% -0.03% higher than that of the quartz boat cleaned by the original quartz device cleaning method.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.

Claims (10)

1. A method for cleaning a quartz device for solar cell preparation is characterized by comprising the following steps:
a) adding mixed liquid medicine of hydrofluoric acid and ozone water into the cleaning tank, heating, and placing the quartz device into the cleaning tank for sealing, soaking and pickling;
b) adding ozone water into a high-temperature rinsing bath, heating, and soaking and cleaning the quartz device soaked and pickled in the step a) in the high-temperature rinsing bath;
c) adding ozone water into the normal-temperature water washing tank, and soaking and washing the quartz device soaked and washed in the step b) in the normal-temperature water washing tank at normal temperature;
d) repeating the step c) until the pH value of the normal-temperature rinsing bath is neutral, and finishing rinsing;
e) and taking out the quartz device after the water washing is finished, and drying to finish the cleaning process of the quartz device.
2. The method for cleaning a quartz device for solar cell production according to claim 1, characterized in that:
the ozone content in the ozone water is 10-30 ppm.
3. The method for cleaning a quartz device for solar cell production according to claim 1 or 2, characterized in that:
in the mixed liquid medicine of hydrofluoric acid and ozone water, the volume ratio of hydrofluoric acid to ozone water is (1-2): (15-20).
4. The method for cleaning a quartz device for solar cell production according to claim 1, characterized in that:
in the step a), the temperature is controlled to be 60-90 ℃ during soaking and pickling, and 40KHz ultrasonic waves and bubbling are used for assisting pickling.
5. The method for cleaning a quartz device for solar cell production according to claim 1, characterized in that:
in the step a), the soaking and pickling time is 15-40 minutes.
6. The method for cleaning a quartz device for solar cell production according to claim 1, characterized in that:
in the step b), the temperature is controlled to be 60-90 ℃ during soaking and cleaning, and 40KHz ultrasonic waves and bubbling are used for assisting cleaning.
7. The method for cleaning a quartz device for solar cell production according to claim 1, characterized in that:
in the step b), the volume of the ozone water is kept to be 200-250L, and the soaking and cleaning time is 10-30 minutes.
8. The method for cleaning a quartz device for solar cell production according to claim 1, characterized in that:
in the step c), bubbling is used for assisting in cleaning during soaking.
9. The method for cleaning a quartz device for solar cell production according to claim 1, characterized in that:
in the step c), the volume of the ozone water is kept to be 200-250L, and the soaking and cleaning time is 10-30 minutes.
10. The method for cleaning a quartz device for solar cell production according to claim 1, characterized in that:
in the step e), the taken quartz device is dried by adopting nitrogen or compressed air.
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