CN110899219A - Device and method for washing impurities of silicon-based powder - Google Patents
Device and method for washing impurities of silicon-based powder Download PDFInfo
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- CN110899219A CN110899219A CN201811531057.9A CN201811531057A CN110899219A CN 110899219 A CN110899219 A CN 110899219A CN 201811531057 A CN201811531057 A CN 201811531057A CN 110899219 A CN110899219 A CN 110899219A
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- 239000011863 silicon-based powder Substances 0.000 title claims abstract description 138
- 238000005406 washing Methods 0.000 title claims abstract description 106
- 239000012535 impurity Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 48
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 35
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001882 dioxygen Inorganic materials 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 15
- 239000000356 contaminant Substances 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000005554 pickling Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims description 42
- 239000002253 acid Substances 0.000 claims description 39
- 239000000126 substance Substances 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 21
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 19
- 239000012498 ultrapure water Substances 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 18
- 239000002699 waste material Substances 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 19
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 239000000843 powder Substances 0.000 description 6
- 229920001774 Perfluoroether Polymers 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000011109 contamination Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005201 scrubbing Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical group C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- -1 Polytetrafluoroethylene Polymers 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000011900 installation process Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1456—Removing acid components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B13/00—Accessories or details of general applicability for machines or apparatus for cleaning
-
- 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
- B08B3/102—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 with means for agitating the liquid
-
- 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
- B08B3/106—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 boiling the liquid
-
- 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
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
Abstract
The invention relates to a device and a method for washing impurities in silicon-based powder. The apparatus of the present invention comprises: a first scrubber in which a first container is provided inside a housing, silicon-based powder, oxygen gas, and a pickling solution are introduced into the first container, a first heating unit is provided on an outer surface of the first container to heat the first container, and a stirrer provided in the housing stirs a solution contained inside the first container to scrub the silicon-based powder 1 time; a second scrubber in which a second container is disposed inside the housing, the silicon-based powder washed in the first scrubber is put into the second container, and a second heating unit is disposed on an outer surface of the second container to wash the silicon-based powder 2 times; an air purifier for filtering the oxygen fed into the first scrubber to generate oxygen from which contaminants are removed; and a washing tower that receives the exhaust gas generated from the first scrubber or the second scrubber and treats oxides contained in the exhaust gas.
Description
Technical Field
The present invention relates to an apparatus and a method for washing impurities of silicon-based powder, and more particularly, to an apparatus and a method for washing impurities of silicon-based powder for washing contaminants formed on the surface of the silicon-based powder and removing the contaminants.
Background
In recent years, strict control has been performed on the purity of silica glass products used in the field of optical communication, semiconductor industry, and the like.
For such high-purity silica glass, the following methods for producing a material for glass articles are being used: a material for producing a glass article, in which a sandy natural quartz powder (alternatively referred to as quartz Sand (Sand)) obtained by pulverizing natural quartz is used as a raw material; and a method for producing a material for glass products using a steam block obtained by causing steam generated by decomposition of silicon tetrachloride in an oxyhydrogen flame to adhere to and grow on a substrate.
The silicon-based powder has heat resistance and chemical resistance exceeding 1000 degrees, and thus is widely used as a raw material for crucibles, washing water tanks, jigs, optical fibers, and optical materials in the semiconductor industry. Among them, as the demand level for impurities is gradually increasing with the progress of high integration of semiconductor products, and the standards for impurity management of silicon-based powders are becoming stricter, and thus, research on a cleaning method capable of removing impurities is under way.
Accordingly, a general technician has been removing impurities by using a hydrofluoric acid cleaning method, a thermal halogen (chlorine) treatment method, or the like, wherein the hydrofluoric acid cleaning method is excellent in an impurity cleaning effect, but the hydrofluoric acid cleaning method may damage a surface of silica to cause a loss of silica powder, and has a disadvantage of high toxicity, thereby complicating a treatment process of flue gas (fume gas), waste liquid, or the like.
Further, in the method of removing impurities by the thermal halogen treatment method, since a highly corrosive chlorine gas is used, facilities related to the impurity treatment need to be made of a corrosion-resistant material, and thus there are problems that a unit cost for installing the facilities is high and an installation process is somewhat complicated, and a process of separating a pipe and pickling and then installing the pipe when cleaning accumulated contaminants is somewhat complicated and a process management is difficult.
Meanwhile, the hydrofluoric acid cleaning method and the thermal halogen treatment method remove impurities using highly toxic substances, and thus, the environmental treatment and management costs are high, and thus, it is difficult to realize mass production or industrialization.
Therefore, in order to solve the problems, there are required a washing method which minimizes the loss of silicon-based powder and the environmental disposal costs at the time of washing and easily removes the contamination of a washing container and a washing method which prevents the introduction of contaminants including foreign materials from the outside to the washing container where washing is additionally performed.
Disclosure of Invention
The invention aims to provide a washing device and a method for washing pollutants formed on the surface of silicon-based powder to remove impurities of the silicon-based powder of the pollutants.
In order to achieve the above object, an apparatus for washing impurities of silicon-based powder according to an embodiment of the present invention may include: a first scrubber in which a first container is provided inside a housing, silicon-based powder, oxygen gas, and a clean pickling solution are introduced into the first container, a first heating unit is provided on an outer surface of the first container to heat the first container, and a stirrer provided in the housing stirs a solution contained inside the first container to scrub the silicon-based powder 1 time; a second scrubber in which a second container is disposed inside a housing, the silicon-based powder washed in the first scrubber is put into the second container, and a second heating unit is disposed on an outer surface of the second container to wash the silicon-based powder 2 times; an air purifier for filtering the oxygen gas introduced into the first scrubber to generate oxygen gas from which contaminants are removed; and a scrubber tower that receives the exhaust gas generated from the first scrubber or the second scrubber and treats oxides contained in the exhaust gas.
In the apparatus for washing impurities in silicon-based powder according to an embodiment of the present invention, the first container may be made of a high-purity synthetic quartz material.
Also, in the apparatus for washing impurities of silicon-based powder according to an embodiment of the present invention, the first heating unit may include a ceramic tape heater.
Also, in the apparatus for washing impurities of silicon-based powder according to an embodiment of the present invention, the second heating unit may include an ultrasonic generator.
Further, in the apparatus for washing impurities of silicon-based powder according to an embodiment of the present invention, the agitator is provided with a motor housing in a housing of the first scrubber, and the agitator further includes: a motor provided inside the motor housing and generating power; a stirring rod extending from the motor, extending into the first container, and rotating by power received from the motor; and a stirring blade provided at an end of the stirring rod and stirring the substance contained in the first container.
Also, in the apparatus for washing foreign substances from silicon-based powder according to an embodiment of the present invention, the agitating bar is provided with a folding part at an inner side, so that the agitating bar is provided in a folding type.
Furthermore, the apparatus for washing impurities from silicon-based powder according to an embodiment of the present invention may further include: a first hose for recovering waste liquid accumulated in the first container and made of a PFA material; and a second hose recovering the silicon-based powder washed 1 time and composed of a PFA material.
In the apparatus for washing impurities from silicon-based powder according to an embodiment of the present invention, the first scrubber may further include: and a temperature measuring unit disposed adjacent to the first container and measuring an external temperature of the first container.
Further, in the apparatus for washing foreign substances from silicon-based powder according to an embodiment of the present invention, the housing of the first scrubber or the housing of the second scrubber may be formed of a plastic material and may be formed in an internally closed configuration.
Furthermore, the apparatus for washing impurities from silicon-based powder according to an embodiment of the present invention may further include: and a filter screen which is provided inside the second container, is made of a material having excellent chemical resistance, and is formed with a mesh of 50 μm, thereby filtering only the silicon-based powder.
Also, the impurity washing method of silicon-based powder according to an embodiment of the present invention may include the steps of: (a) injecting silicon-based powder, acid cleaning solution and oxygen into a first container, and stirring a substance contained in the first container by a stirrer while heating the first container by a first heating unit, thereby washing the silicon-based powder for 1 time; (b) sequentially recovering waste liquid and silicon-based powder from the first container, and injecting the silicon-based powder into a second container; (c) injecting ultra-pure water into the second container, and washing the silicon-based powder for 2 times through a second heating unit arranged outside the second container; (d) and removing the moisture contained in the silicon-based powder and recovering the silicon-based powder.
Also, according to the impurity washing method of the silicon-based powder according to an embodiment of the present invention, oxygen gas for removing contaminants in an air purifier may be used in the (a) step.
In the method for washing impurities in a silicon-based powder according to an embodiment of the present invention, the acid-washing cleaning solution may be any one of hydrochloric acid, sulfonic acid, and nitric acid of electronic grade or higher.
In the impurity washing method of the silicon-based powder according to an embodiment of the present invention, the concentration of the acid cleaning solution may range from 2 to 20 w%.
In the impurity washing method of the silicon-based powder according to an embodiment of the present invention, hydrogen peroxide may be added to the acid cleaning solution at a concentration of less than 2 w%.
Also, in the impurity washing method of silicon-based powder according to an embodiment of the present invention, the acid cleaning solution may be heated at a temperature ranging from 40 degrees to not reaching a boiling point for 1 to 3 hours.
In the method for washing impurities in the silicon-based powder according to an embodiment of the present invention, the silicon-based powder, the acid cleaning solution, and the oxygen gas contained in the first container may be stirred 2 or more times in the step (a). Since only 1 stirring pass brings about a problem of poor mixing effect, at least 2 stirring passes are required (regardless of the rotation speed, stirring speed parameters, and the like).
Further, according to the impurity washing method of the silicon-based powder of the embodiment of the present invention, in the step (b), the silicon-based powder may be recovered through the second hose after the waste liquid of the acid cleaning solution is recovered through the first hose.
Further, according to the impurity washing method for silicon-based powder of an embodiment of the present invention, after the waste liquid of the acid cleaning liquid and the silicon-based powder are recovered in the step (b), ultrapure water may be injected into the first container to wash the first container.
Also, in the impurity washing method of silicon-based powder according to an embodiment of the present invention, the ultrapure water may be injected in a range of 2 to 3 times the capacity of the first container, thereby washing the first container.
In the method of washing impurities in the silicon-based powder according to an embodiment of the present invention, the first container may be washed with nitric acid having a concentration of less than 10 w% while the step of removing impurities from the silicon-based powder is continuously repeated.
In the method for washing impurities in the silicon-based powder according to the embodiment of the present invention, the conductivity may be measured for the 2-time washing in a cycle of 10 minutes, and the 2-time washing may be repeatedly performed until the conductivity of the ultrapure water is less than 0.5 μ s/cm.
According to an embodiment of the present invention, it is possible to prevent a portion of the powder from being lost when washing the silicon-based powder, minimize environmental treatment costs, and prevent contaminants including foreign substances from flowing into the interior of the scrubber.
Drawings
Fig. 1 is a schematic view illustrating an apparatus for washing impurities of silicon-based powder according to an embodiment of the present invention.
Fig. 2 is a side view of an air purifier and a first scrubber showing a device for scrubbing foreign substances of silicon-based powder according to an embodiment of the present invention.
Fig. 3 is a side view illustrating a first scrubber, a second scrubber, and a washing tower of the apparatus for washing impurities of silicon-based powder according to an embodiment of the present invention.
Fig. 4 is a block diagram illustrating an impurity washing method of a silicon-based powder according to an embodiment of the present invention.
Description of the symbols
100: the first scrubber 110: outer casing
110 a: inner space 111: exhaust pipe
113: t-pipe 115: air supply pipe
120: the stirrer 121: motor with a stator having a stator core
122: the motor case 123: stirring rod
124: folding portion 125: stirring wing
130: first container 131: first heating unit
140: first hose 150: second flexible pipe
200: the second scrubber 210: outer casing
210 a: inner space 211: exhaust pipe
220: second container
221: the filter screen 223: second heating unit
300: the air purifier 400: controller
500: the washing tower 510: pump section
511: the gas supply pipe 520: storage part
530: nozzle 540: exhaust pipe
Detailed Description
Hereinafter, an embodiment of the present invention will be described in detail with reference to the accompanying drawings.
An apparatus for washing impurities of silicon-based powder according to an embodiment of the present invention includes a first scrubber 100 for washing silicon-based powder 1 time, a second scrubber for washing silicon-based powder 2 times, an air purifier 300 for generating purified oxygen, and a washing tower 500 for treating oxides generated in the first scrubber and the second scrubber 200.
The first scrubber 100 is constructed as follows: the interior of the outer case 110 is provided with a space 110a, the interior space 110a is provided with a first container 130 and a first heating unit 131, and the stirrer 120 is disposed to be directed from the outside to the inside of the outer case 110.
The housing 110 is formed of a plastic material and has an internally closed structure, so that it is possible to prevent foreign substances from penetrating into the internal space 110a from the outside and to prevent foreign substances existing outside from being stirred with the silicon-based powder when the silicon-based powder is washed.
Also, the housing 110 is provided with an exhaust pipe 111 and an air supply pipe 115 at one side, for example, an upper portion in the drawing, and oxygen generated from the air cleaner 300 is supplied to the first scrubber 100 through the air supply pipe 115, or oxide generated after 1 time of scrubbing in the first scrubber 100 may be discharged through the exhaust pipe 111.
The air supply pipe 115 may be provided with a filter part (not shown) including a primary filter and a hepa filter inside to prevent inflow of particles in order to prevent oxygen purified from the air purifier 300 from being contaminated during movement.
The housing 110 is provided at a side thereof with a stirrer 120 so that the substance received in the first container can be stirred.
The stirrer 120 is provided obliquely to one side of the housing 110, for example, obliquely to the left side with reference to fig. 2, and is provided obliquely to one side, for example, the left side in the drawing, and the stirring rod 123 is provided to penetrate through the inside so as to be positioned inside the first container 130, and is configured to stir the substance contained in the first container 130.
The stirrer 120 has a structure in which a motor 121 is provided to protrude outside the housing 110, a motor case 122 is provided around the motor 121, and a stirring rod 123 is provided to extend from the motor 121 so that the stirring rod 123 can be rotated by power received from the motor 121.
The stirring rod 123 is made of a material selected from PTFE (Polytetrafluoroethylene) and PFA (PerFluoroAlkoxy) having a heat resistance temperature of 200 degrees or higher among fluororesins, one end portion thereof is connected to the motor 121, the other end portion thereof is provided with a stirring blade 125, the stirring blade 125 is provided so as to be positioned inside the first container 130, and the stirring rod 123 is configured to be capable of stirring the substance contained in the first container 130 by the stirring blade 125.
The stirring rod 123 may be formed in a foldable manner by providing a folding portion 124 at a predetermined position.
In order to prevent contamination due to elution of impurities from the acid cleaning solution, the first vessel 130 is preferably made of a high-purity material having heat resistance, and in the present invention, high-purity synthetic quartz or fluorine resin may be used.
The first container 130 may contain a substance (in the present invention, the acid cleaning solution, the silicon-based powder, and the purified oxygen gas) therein, and then the silicon-based powder may be washed 1 time by heating and stirring, and the first container 130 may be heated by a first heating unit 131 provided outside.
The first heating means 131 is configured to heat the material contained in the first container 130 to facilitate the washing of the silicon-based powder, and when the first heating means 131 is provided at the side and the lower portion of the first container 130, the first container 130 is uniformly heated.
Further, the first heating unit 131 may be preferably configured by any one of a heater lined with a fluororesin or a heater made of a ceramic material, but in the present invention, a belt heater made of a ceramic material is used in order to prevent contamination due to elution of impurities while a part of the first heating unit 131 is deteriorated due to continuous use of the first heating unit 131.
Meanwhile, the first container 130 is additionally provided with a temperature measuring part (not shown) between the first heating unit 131, so that the temperature of a space formed between the first container 130 and the first heating unit 131 can be measured.
The first scrubber 100 may sequentially collect the waste liquid of the acid cleaning solution and the silicon-based powder stored in the first tank 130 after 1 time of washing in the first tank 130, and may further include a first hose 140 for collecting the waste liquid of the acid cleaning solution and a second hose 150 for collecting the silicon-based powder.
The first and second hoses 140 and 150 are provided to penetrate from the outside of the housing 110 to the inside of the housing 110, and are configured to be able to collect waste liquid of the pickling solution and the silicon-based powder stored in the first container 130 to the outside, and the first and second hoses 140 and 150 are made of PFA material having excellent chemical resistance and heat resistance and a heat resistance temperature of 250 degrees or more.
In addition, the second scrubber 200 is provided with a space 210a inside the housing 210, is provided with a second container 220 and a second heating unit 223 in the inner space 210a, and can scrub the silicon-based powder, which has been scrubbed 1 time in the first scrubber 100, 2 times.
The housing 210 is formed of a plastic material and has an internally closed structure, so that it is possible to prevent foreign substances from penetrating into the internal space 210a from the outside and to prevent foreign substances existing outside from being stirred with the silicon-based powder when the silicon-based powder is washed.
Also, the housing 210 is provided with an exhaust pipe 211 at one side, for example, an upper portion in the drawing, so that the oxide generated after the second scrubber 200 completes 2 washes can be exhausted through the exhaust pipe 211.
Here, the exhaust pipe 111 provided in the first scrubber 100 and the exhaust pipe 211 provided in the second scrubber 200 are connected to each other by a T-pipe 113, and the oxide formed in the first scrubber 100 and the second scrubber 200 can be moved to the cleaning tower 500.
The second container 220 is provided in the second scrubber, a second heating unit 223 is provided on one surface of the second container 220, for example, at the lower portion in the drawing, and the second heating unit 223 heats the second container 220 to heat the substance contained in the second container 220.
The second container 220 is made of the same material as the first container 130, i.e., a high purity synthetic quartz material, and is configured to easily recover the silica-based powder by filtering the silica-based powder by providing a filter 221 therein.
The filter 221 is provided inside the second container 220, and is configured to be movable up and down, and the controller 400 operates the filter 221.
The mesh 221 is made of any one of PE, PP, and fluororesin having excellent chemical resistance, and is configured to contain only silica-based powder in the mesh 221 by forming a mesh of 50 μm.
Further, since the second container 220 is configured to be movable up and down by the controller 400, the silicon-based powder can be easily recovered after 2 times of washing in the second container 220.
The second heating unit 223 is composed of an ultrasonic generator generating ultrasonic waves, and the ultrasonic waves generated from the ultrasonic generator are continuously transferred to the second container 220, so that ultrasonic washing can be performed on the silicon-based powder.
Further, the washing tower 500 is configured to receive the exhaust gas generated from the first scrubber 100 and the second scrubber 200 and then treat the oxides contained in the exhaust gas, and in the present invention, the oxides generated when the silicon-based powder is washed are contained in the exhaust gas, and for example, the oxides (hydrochloric acid, nitric acid, sulfuric acid) generated in the first scrubber 100 and the oxides remaining after 1 time of washing in the second scrubber 200 are washed 2 times and the oxides remaining after 2 times of washing in the second scrubber 200 are contained in the exhaust gas.
The washing tower 500 is configured such that the exhaust gas generated from the first scrubber 100 and the second scrubber 200 can easily flow into the washing tower 500 through the pump unit 510, and a separate air supply pipe 511 is provided between the pump unit 510 and the washing tower 500.
The washing tower 500 is structured as follows: a container 520 for containing oxides contained in the exhaust gas is provided inside, spray pipes 530 for spraying water are arranged above the container 520, and the oxides contained in the container 520 are treated by spraying water through the spray heads 530.
Exhaust gas generated when the oxides are treated is discharged through the exhaust pipe 540.
Further, the method for washing impurities of silicon-based powder according to an embodiment of the present invention includes a step of washing the silicon-based powder 1 time by the first washer 100 (S100), a step of injecting the silicon-based powder into the second washer 200 (S200), a step of washing the silicon-based powder 2 times by the second washer 200 (S300), and a step of removing moisture contained in the silicon-based powder and recovering (S400).
In the step of performing the washing 1 time in the first scrubber 100, the silicon-based powder, the acid cleaning solution, and the oxygen gas are sequentially injected into the first container 130, and the first heating unit 131 heats the first container 130 while stirring the silicon-based powder, the acid cleaning solution, and the oxygen gas by the stirrer 120 provided to the first scrubber 100, thereby performing the washing 1 time on the silicon-based powder.
Here, the oxygen gas injected into the first scrubber 100 is purified oxygen gas from which contaminants are removed in the air purifier 300, and impurities can be prevented from flowing into the silicon-based powder by purifying the oxygen gas.
The acid cleaning solution may be injected by selecting any one of hydrochloric acid, sulfuric acid and nitric acid of electronic grade or more, and in the present invention, hydrochloric acid may be selected and used in consideration of the harmfulness of the reactive flue gas during heating.
The acid concentration of the acid cleaning solution is set in the range of 2 to 20 w%, and the washing effect is improved as the acid concentration increases, but the washing effect is not more than 20 w% after exceeding 20 w% and the washing time is long, so that it is preferably set to be within 20 w%.
Further, if the acid concentration of the acid cleaning solution exceeds 10 w%, it is selected as a harmful chemical in the object of chemical management law management, and therefore, it is preferable to set it to be less than 10 w%, and in the present invention, it is preferable to set it to be in the range of 5 to 9 w%.
Further, if hydrogen peroxide is added to the acid cleaning solution, the metal components remaining in the acid cleaning solution can be removed, and it is preferably added in an amount of less than 2 w% in view of the effectiveness and the problem of drainage treatment.
Such an acid cleaning solution can be used for 1 washing of the silicon-based powder by heating for 1 to 3 hours at a temperature ranging from 40 degrees to not reaching the boiling point.
That is, in the 1-time washing step S100, the silicon-based powder, the acid cleaning solution, and the purified oxygen gas stored in the first container are heated and stirred to be washed, and 2 or more times of stirring is performed to facilitate stirring of the silicon-based powder with the acid cleaning solution and the oxygen gas.
After the washing step S100 of step 1 is performed, the waste liquid of the acid cleaning solution and the silicon-based powder are collected from the first container 130 through the first hose 140 and the second hose 150 (S200), the waste liquid of the acid cleaning solution is collected exclusively through the first hose 140, and the silicon-based powder is collected exclusively through the second hose 150, thereby preventing the waste liquid remaining in the hoses from being included in the silicon-based powder in advance.
The first container 130 injects ultrapure water to the first container 130 after recovering the waste liquid of the acid cleaning solution and the silicon-based powder, respectively, to wash the first container, thereby preventing impurities generated when 1 washing is performed from contaminating the first container 130 in advance, and can inject ultrapure water of 2 to 3 times the volume of the first container 130, thereby washing the first container in a sufficient amount.
However, when the first container 130 continuously repeats the impurity removal process of the silicon-based powder, it is preferable to wash with nitric acid having a concentration of less than 10 w% instead of ultra pure water, thereby washing the impurities accumulated on the inner surface of the first container 130.
Further, after the silicon-based powder is injected into the second container 220 and the ultra-pure water is additionally injected, ultrasonic cleaning is performed by the second heating unit 223 and 2 times of cleaning of impurities remaining in the silicon-based powder is performed (S300).
After the silicon-based powder and the ultrapure water having been washed 1 time are stored in the second container 220, acid radicals remaining in the silicon-based powder (more specifically, acid radicals remaining after 1-time washing with an acid washing solution) and impurities eluted from the silicon-based powder are rinsed with ultrapure water, and the acid radicals and the impurities are washed.
Rinsing ultra pure water rinsed was discharged every predetermined time while ultrasonic washing was performed, and water was discharged at intervals of 10 minutes in the present invention.
The conductivity of the ultrapure water after the rinsing is measured, the silicon-based powder is repeatedly rinsed until the conductivity of the ultrapure water decreases to 0.5 μ S/cm or less, and the moisture (ultrapure water) contained in the silicon-based powder is removed when the conductivity of the ultrapure water decreases to 0.5 μ S/cm or less, and the silicon-based powder is recovered from the second container 220 (S400).
When removing moisture contained in the silicon-based powder, the moisture contained in the silicon-based powder is removed by the sieve 221, and the sieve 221 is made in a size of 50 μm, thereby being configured to be able to filter only the silicon-based powder.
The above description is only an exemplary illustration of the technical idea of the present invention, and a person having a basic knowledge in the technical field to which the present invention belongs can realize various modifications and variations within a range not departing from the essential characteristics of the present invention. Therefore, the embodiments disclosed in the present invention are only for illustration and not intended to limit the technical idea of the present invention, and the scope of the technical idea of the present invention is not limited by the embodiments described above. The scope of the present invention should be construed based on the claims, and it should be construed that all technical ideas within the equivalent scope are included in the scope of the present invention.
Claims (18)
1. An apparatus for washing impurities from silicon-based powder, comprising:
a first scrubber in which a first container is provided inside a housing, silicon-based powder, oxygen gas, and a clean pickling solution are introduced into the first container, a first heating unit is provided on an outer surface of the first container to heat the first container, and a stirrer provided in the housing stirs the solution contained in the first container to scrub the silicon-based powder 1 time;
a second scrubber in which a second container is disposed inside a housing, the silicon-based powder washed in the first scrubber is put into the second container, and a second heating unit is disposed on an outer surface of the second container to wash the silicon-based powder 2 times;
an air purifier for filtering the oxygen gas introduced into the first scrubber to generate oxygen gas from which contaminants are removed; and
and a washing tower which receives the exhaust gas generated from the first scrubber or the second scrubber and treats oxides contained in the exhaust gas.
2. The apparatus for washing impurities of silicon-based powder according to claim 1,
the first heating unit includes a ceramic band heater.
3. The apparatus for washing impurities of silicon-based powder according to claim 1,
the second heating unit includes an ultrasonic generator.
4. The apparatus for washing impurities of silicon-based powder according to claim 1,
the agitator is in the casing of first scrubber is provided with motor housing, the agitator still includes:
a motor provided inside the motor housing and generating power;
a stirring rod extending from the motor, extending into the first container, and rotating by power received from the motor;
and a stirring blade provided at an end of the stirring rod and stirring the substance contained in the first container.
5. The apparatus for washing impurities of silicon-based powder according to claim 4,
the stirring rod is provided with a folding portion at an inner side so that the stirring rod is prepared in a folding type.
6. The apparatus for washing impurities of silicon-based powder according to claim 1, further comprising:
a first hose for recovering waste liquid accumulated in the first container and made of a PFA material;
and a second hose recovering the silicon-based powder washed 1 time and composed of a PFA material.
7. The apparatus for washing impurities of silicon-based powder according to claim 1,
the first scrubber further comprises: and a temperature measuring unit disposed adjacent to the first container and measuring an external temperature of the first container.
8. An impurity washing method of silicon-based powder is characterized by comprising the following steps:
(a) injecting silicon-based powder, acid cleaning solution and oxygen into a first container, and stirring a substance contained in the first container by a stirrer while heating the first container by a first heating unit, thereby washing the silicon-based powder for 1 time;
(b) sequentially recovering waste liquid and silicon-based powder from the first container, and injecting the silicon-based powder into a second container;
(c) injecting ultra-pure water into the second container, and washing the silicon-based powder for 2 times through a second heating unit arranged outside the second container;
(d) and removing the moisture contained in the silicon-based powder and recovering the silicon-based powder.
9. The impurity washing method for silicon-based powder according to claim 8,
the acid cleaning solution is any one of hydrochloric acid, sulfonic acid and nitric acid with the electronic grade or above.
10. The impurity washing method for silicon-based powder according to claim 8,
the concentration range of the acid cleaning solution is 2-20 w%.
11. The impurity washing method for silicon-based powder according to claim 8,
hydrogen peroxide with the concentration of less than 2w percent is added into the acid cleaning solution.
12. The impurity washing method for silicon-based powder according to claim 8,
the acid cleaning solution is heated for 1 to 3 hours in the temperature range of 40 ℃ to the boiling point.
13. The impurity washing method for silicon-based powder according to claim 8,
in the step (a), the silicon-based powder, the acid cleaning solution, and the oxygen gas are stirred in the first container for 2 or more cycles.
14. The impurity washing method for silicon-based powder according to claim 8,
and (b) recovering the silicon-based powder through a second hose after recovering the waste liquid of the acid cleaning solution through the first hose.
15. The impurity washing method for silicon-based powder according to claim 8,
and (c) after recovering the waste liquid of the acid cleaning liquid and the silicon-based powder in the step (b), injecting ultrapure water into the first container to wash the first container.
16. The impurity washing method for silicon-based powder according to claim 15,
injecting the ultrapure water in a range of 2 to 3 times the capacity of the first container, thereby washing the first container.
17. The impurity washing method for silicon-based powder according to claim 15,
the first container is washed with nitric acid having a concentration of less than 10 w% while continuously repeating the impurity removal process of the silicon-based powder.
18. The impurity washing method for silicon-based powder according to claim 8,
for the 2-time washing, the conductivity is measured in 10 minutes as a period until the conductivity of the ultrapure water reaches 0.5 μ s/cm or less, and the 2-time washing is repeatedly performed.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020180111488A KR102110202B1 (en) | 2018-09-18 | 2018-09-18 | Apparatus and method for impurity removal of silica-based powder |
| KR10-2018-0111488 | 2018-09-18 |
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| Publication Number | Publication Date |
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| CN110899219A true CN110899219A (en) | 2020-03-24 |
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| CN201811531057.9A Withdrawn CN110899219A (en) | 2018-09-18 | 2018-12-14 | Device and method for washing impurities of silicon-based powder |
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| Country | Link |
|---|---|
| JP (1) | JP6714678B2 (en) |
| KR (1) | KR102110202B1 (en) |
| CN (1) | CN110899219A (en) |
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| CN113082809B (en) * | 2021-04-09 | 2022-12-16 | 东方电气集团科学技术研究院有限公司 | Bubbling stirring type nano powder cleaning and filtering device and method |
| CN113275121A (en) * | 2021-06-11 | 2021-08-20 | 四川敏田科技发展有限公司 | High-purity quartz sand manufacturing system and manufacturing method |
| KR102602595B1 (en) | 2021-11-22 | 2023-11-16 | (주)선영시스텍 | Metal powder washing machine |
| CN115350999A (en) * | 2022-08-24 | 2022-11-18 | 米易锦秀机械制造有限公司 | Titanium white powder tailings washing tank |
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| JPH10226510A (en) * | 1997-02-07 | 1998-08-25 | Toho Aen Kk | Preliminary treatment of metal silicon powder |
| CN101121169A (en) * | 2007-09-10 | 2008-02-13 | 张家港市超声电气有限公司 | Pickling groove in silicon material cleaning device |
| CN101181997A (en) * | 2007-11-29 | 2008-05-21 | 晶湛（南昌）科技有限公司 | Method for preparing metallic silicon material |
| CN101748492A (en) * | 2008-11-28 | 2010-06-23 | 三菱麻铁里亚尔株式会社 | Apparatus and method for washing polycrystalline silicon |
| KR20130071186A (en) * | 2011-12-20 | 2013-06-28 | 주식회사 포스코 | Apparatus and method for refining silicon |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100489931B1 (en) * | 2002-01-29 | 2005-05-17 | 한국지질자원연구원 | High purity careful manufacture method of natural silica |
| KR100719164B1 (en) * | 2005-05-04 | 2007-05-17 | 에이비앤씨코리아(주) | The device for washing gravels using construction |
| KR20130086754A (en) * | 2012-01-26 | 2013-08-05 | (주)에스피에이시티 | Method for cleaning semiconductor and display panel during manufacturing process of semiconductor and display panel and apparatus thereof |
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2018
- 2018-09-18 KR KR1020180111488A patent/KR102110202B1/en active IP Right Grant
- 2018-12-10 JP JP2018230692A patent/JP6714678B2/en active Active
- 2018-12-14 CN CN201811531057.9A patent/CN110899219A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10226510A (en) * | 1997-02-07 | 1998-08-25 | Toho Aen Kk | Preliminary treatment of metal silicon powder |
| CN101121169A (en) * | 2007-09-10 | 2008-02-13 | 张家港市超声电气有限公司 | Pickling groove in silicon material cleaning device |
| CN101181997A (en) * | 2007-11-29 | 2008-05-21 | 晶湛（南昌）科技有限公司 | Method for preparing metallic silicon material |
| CN101748492A (en) * | 2008-11-28 | 2010-06-23 | 三菱麻铁里亚尔株式会社 | Apparatus and method for washing polycrystalline silicon |
| KR20130071186A (en) * | 2011-12-20 | 2013-06-28 | 주식회사 포스코 | Apparatus and method for refining silicon |
Also Published As
| Publication number | Publication date |
|---|---|
| JP6714678B2 (en) | 2020-06-24 |
| KR102110202B1 (en) | 2020-06-09 |
| JP2020045271A (en) | 2020-03-26 |
| KR20200032791A (en) | 2020-03-27 |
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