CN114534886A - Electronic grade polycrystalline silicon thermal crushing heating device, heating method and crushing device - Google Patents
Electronic grade polycrystalline silicon thermal crushing heating device, heating method and crushing device Download PDFInfo
- Publication number
- CN114534886A CN114534886A CN202210135546.2A CN202210135546A CN114534886A CN 114534886 A CN114534886 A CN 114534886A CN 202210135546 A CN202210135546 A CN 202210135546A CN 114534886 A CN114534886 A CN 114534886A
- Authority
- CN
- China
- Prior art keywords
- heating
- bin
- electronic grade
- heating chamber
- polycrystalline silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000010438 heat treatment Methods 0.000 title claims abstract description 183
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229920005591 polysilicon Polymers 0.000 claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 23
- 230000001681 protective effect Effects 0.000 claims abstract description 12
- 238000012546 transfer Methods 0.000 claims abstract description 8
- 238000013467 fragmentation Methods 0.000 claims description 23
- 238000006062 fragmentation reaction Methods 0.000 claims description 23
- 239000010453 quartz Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 10
- 239000010963 304 stainless steel Substances 0.000 claims description 7
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 7
- 239000004809 Teflon Substances 0.000 claims description 4
- 229920006362 Teflon® Polymers 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000013021 overheating Methods 0.000 abstract description 2
- 230000007306 turnover Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 19
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 239000002210 silicon-based material Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 238000004227 thermal cracking Methods 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
- B02C19/186—Use of cold or heat for disintegrating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses an electronic grade polysilicon thermal crushing heating device, a heating method and a crushing device, wherein the device comprises: a transfer unit; the heating chamber is provided with bin openings on two opposite side faces of the heating chamber, the conveying unit penetrates through the bin openings movably, bin doors are arranged at the bin openings, the heating chamber forms a closed space when the bin doors are closed, heaters and temperature detectors are arranged on the inner wall of the heating chamber, and vacuumizing ports and protective gas inlets are further formed in the wall of the heating chamber. The polycrystalline silicon rod passes through the automatic business turn over heating cabinet of accomplishing of conveying unit, and polycrystalline silicon rod is in the in-process of accomplishing the heating, except conveying unit, has not contacted other material, and single contact source has avoided the problem of external pollution source, has guaranteed heating efficiency simultaneously.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to an electronic grade polycrystalline silicon thermal crushing and heating device, a heating method and a crushing device.
Background
Polycrystalline silicon is a basic material used in the electronics industry and is also a main raw material for silicon wafer production. The production of electronic grade polysilicon in China is in the starting stage, and except the introduction of core production devices, other production devices are different from enterprises. The post-treatment section is the last processing procedure of the production of electronic grade polysilicon, and the main production task is to carry out crushing processing on the polysilicon rod produced in the reduction hydrogenation section to generate a final product, so the post-treatment is called as post-treatment. Because the requirement on the purity of the electronic grade polysilicon is extremely high, the post-treatment processing process is easy to pollute, the post-treatment process of the electronic grade polysilicon has no reference for a mature design scheme at present, and various production plants are gradually improved after continuous exploration, supplement and improvement. Therefore, manufacturers at home and abroad are improving the silicon material crushing in recent years, and the technical scheme of heating, quickly cooling and then crushing polycrystalline silicon is proposed in the prior art, but the prior art can generate pollution in the heating process and needs further improvement.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention aims to provide an electronic grade polycrystalline silicon thermal crushing and heating device, a heating method and a crushing device. The polycrystalline silicon rod passes through the automatic business turn over heating cabinet of accomplishing of conveying unit, and polycrystalline silicon rod is in the in-process of accomplishing the heating, except conveying unit, has not contacted other material, and single contact source has avoided the problem of external pollution source, has guaranteed heating efficiency simultaneously.
In a first aspect of the invention, an electronic grade polysilicon thermal fragmentation heating apparatus is presented. According to an embodiment of the invention, the electronic grade polysilicon thermal fragmentation heating apparatus comprises:
a transfer unit;
the heating chamber is provided with bin openings on two opposite side faces of the heating chamber, the conveying unit penetrates through the bin openings movably, bin doors are arranged at the bin openings, the heating chamber forms a closed space when the bin doors are closed, heaters and temperature detectors are arranged on the inner wall of the heating chamber, and vacuumizing ports and protective gas inlets are further formed in the wall of the heating chamber.
According to the electronic-grade polycrystalline silicon thermal-breaking heating device provided by the embodiment of the invention, the polycrystalline silicon rod to be heated is conveyed into the heating bin through the conveying unit, the bin door is closed, the heating bin forms a closed space, air in the heating bin body is evacuated through the vacuumizing port, and after the evacuation, protective gas is filled to block oxygen, so that the electronic-grade polycrystalline silicon rod is prevented from being oxidized due to high temperature in the heating process; starting a heater to heat the polycrystalline silicon rod in the heating bin, and monitoring the temperature in the heating bin through a temperature detector; and after the heating is finished, opening the bin door, and conveying the heated polycrystalline silicon rod out of the heating bin through the conveying unit. Therefore, the polycrystalline silicon rod automatically passes in and out of the heating bin through the conveying unit, and the polycrystalline silicon rod is not contacted with other substances except the conveying unit in the heating process, so that the problem of an external pollution source is avoided due to the single contact source, and the heating efficiency is ensured.
In addition, the electronic grade polysilicon thermal fragmentation heating device according to the above embodiment of the present invention may also have the following additional technical features:
in some embodiments of the present invention, the conveying unit includes a gear and a conveyor belt, the conveyor belt is disposed on the gear, and an upper surface of the bottom wall of the heating chamber is provided with a tooth mark corresponding to the gear.
In some embodiments of the present invention, the conveyor belt comprises a plurality of conveying pieces, the length of a single conveying piece along the length direction of the conveying unit is 8-12cm, and the distance between adjacent conveying pieces is 1.5-2.5 cm.
In some embodiments of the present invention, the material of the conveyor belt is quartz, and the quartz is SiO2The mass content of the gear is not less than 99.99 percent, and the material of the gear is 304 stainless steel.
In some embodiments of the invention, the door is sealed from the hatch by a sealing layer.
In some embodiments of the present invention, the sealing layer is made of teflon.
In some embodiments of the present invention, the wall of the heating chamber comprises two layers, the outer layer is made of 304 stainless steel, the inner layer is made of quartz, and SiO in the quartz2The mass content of (A) is not less than 99.99%.
In some embodiments of the invention, a chilled water coil is disposed between the outer layer and the inner layer.
In some embodiments of the present invention, a cylinder is further disposed on a side wall of the heating chamber, and the cylinder is connected to the chamber door through a connecting rod.
In some embodiments of the invention, a nanofilter is provided at the shielding gas inlet.
In some embodiments of the invention, the purity of the shielding gas entering the heating chamber is no less than 99.999%.
In some embodiments of the present invention, the length of the polysilicon rod to be heated is 300-.
In a second aspect of the invention, the invention provides a method for heating a polysilicon rod by using the electronic grade polysilicon thermal cracking heating device of the above embodiment. According to an embodiment of the invention, the method comprises:
(1) opening a bin door, conveying the polycrystalline silicon rod to be heated into a heating bin by adopting a conveying unit, and closing the bin door to form a closed space in the heating bin;
(2) evacuating air in the heating bin through a vacuumizing port, and filling protective gas;
(3) starting a heater, and heating the polysilicon rod to 500-1000 ℃;
(4) and opening the bin door, and conveying the heated polycrystalline silicon rods out of the heating bin through the conveying unit.
According to the heating method of the embodiment of the invention, the polycrystalline silicon rod to be heated is conveyed into the heating bin through the conveying unit, the bin door is closed, the heating bin forms a closed space, air in the heating bin body is evacuated through the vacuumizing port, and protective gas is filled after the evacuation is finished to block oxygen so as to prevent the electronic-grade polycrystalline silicon rod from being oxidized due to high temperature in the heating process; starting a heater to heat the polycrystalline silicon rod in the heating bin, and monitoring the temperature in the heating bin through a temperature detector; and after the heating is finished, opening the bin door, and conveying the heated polycrystalline silicon rod out of the heating bin through the conveying unit. Therefore, the polycrystalline silicon rod automatically passes in and out of the heating bin through the conveying unit, and the polycrystalline silicon rod is not contacted with other substances except the conveying unit in the heating process, so that the problem of an external pollution source is avoided due to the single contact source, and the heating efficiency is ensured.
In addition, the method according to the above embodiment of the present invention may also have the following additional technical features:
in some embodiments of the invention, step (3) comprises the steps of: starting a heater, and heating the polysilicon rod to 350-450 ℃ at a heating speed of 15-20 ℃/min; heating the polysilicon rod to 500-1000 ℃ at a heating speed of 25-35 ℃/min.
In a third aspect of the invention, an electronic grade polysilicon thermal fragmentation device is presented. According to an embodiment of the present invention, the electronic grade polysilicon thermal fragmentation device has the electronic grade polysilicon thermal fragmentation heating device described in the above embodiment. Therefore, in the process that the polycrystalline silicon rod is heated in the electronic-grade polycrystalline silicon thermal crushing device, other substances are not contacted except the conveying unit, and a single contact source is adopted, so that the problem of an external pollution source is avoided, and the heating efficiency is ensured.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a cross-sectional view of an electronic grade polysilicon thermal break heater according to one embodiment of the present invention;
fig. 2 is a front view of an electronic grade polysilicon thermal break heater according to yet another embodiment of the invention.
Labeling: 10-conveying unit, 20-heating bin, 11-conveying belt, 12-gear, 21-bin gate, 22-sealing layer, 23-connecting rod, 24-heater, 25-temperature detector, 26-vacuumizing port, 27-protective gas inlet, 28-nano filter, 29-bin port and 30-support.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", "radial", "circumferential", and the like, indicate orientations and positional relationships based on the orientations and positional relationships shown in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of the feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
The invention provides an electronic grade polysilicon thermal crushing and heating device, which comprises the following components with reference to the attached figures 1 and 2: a transfer unit 10; heating chamber 20, be equipped with door 29 on two relative sides of heating chamber 20, conveying unit 10 passes through door 29 is movably run through heating chamber 20, door 29 department is equipped with door 21, when door 21 closes heating chamber 20 forms the enclosure space, be equipped with heater 24 and temperature detector 25 on heating chamber 20's the inner wall, just still be equipped with evacuation mouth 26 and protective gas entry 27 on the heating chamber wall. Therefore, the polycrystalline silicon rod to be heated is conveyed into the heating bin 20 through the conveying unit 10, the bin door 21 is closed, the heating bin 20 forms a closed space, air in the heating bin 20 is exhausted through the vacuumizing port 26, and after the air is exhausted, protective gas is filled to block oxygen so as to prevent the electronic-grade polycrystalline silicon rod from being oxidized due to high temperature in the heating process; starting the heater 24 to heat the polysilicon rod in the heating bin 20, and simultaneously monitoring the temperature in the heating bin 20 through the temperature detector 25; after the heating is completed, the bin gate 21 is opened, and the heated polysilicon rod is transferred out of the heating bin 20 by the transfer unit 10. Therefore, the polycrystalline silicon rod automatically enters and exits the heating bin 20 through the conveying unit 10, and in the process of heating the polycrystalline silicon rod, other substances are not contacted except the conveying unit 10, and the polycrystalline silicon rod is in single contact source, so that the problem of external pollution sources is avoided, and meanwhile, the heating efficiency is ensured.
The electronic grade polysilicon thermal fragmentation heating apparatus according to embodiments of the present invention is described in further detail below.
According to some embodiments of the present invention, referring to fig. 1, the conveying unit 10 includes a gear 12 and a conveyor belt 11, the conveyor belt 11 is disposed on the gear 12, and the upper surface of the bottom wall of the heating chamber 20 is provided with a tooth mark corresponding to the gear 12. It will be understood that the teeth on the upper surface of the bottom wall of the heating chamber 20 are engaged with the gear 12 of the conveyor unit 10, and the gear 12 is moved forward by interaction with the teeth under the action of a motor (not shown in the figures), so as to move the conveyor belt 11 forward. The transfer unit 10 rotates around the bottom wall of the heating chamber 20.
According to some embodiments of the present invention, the conveyor belt 11 comprises a plurality of conveying pieces, a length of a single conveying piece along a length direction of the conveying unit 10 is 8-12cm, and a distance between adjacent conveying pieces is 1.5-2.5cm, so that the conveyor belt 11 is divided into a plurality of units, and a certain distance is provided between adjacent units, which further facilitates the rotation of the conveyor belt 11 around the bottom wall of the heating chamber 20 under the driving of the gear 12. It will be appreciated that the conveyor belt 11 is typically made of a relatively rigid material, such as quartz, and that without dividing the conveyor belt 11 into a plurality of conveyor segments, the conveyor belt 11 cannot flex and thus cannot rotate about the bottom wall of the heating chamber 20.
In the embodiment of the present invention, the material of the conveyor belt 11 is not particularly limited, and may be arbitrarily selected by those skilled in the art according to actual needs, as long as the conveyor belt 11 formed of the material is not liable to cause contamination to the polysilicon rod placed thereon at a high temperature, as a specific example, the material isThe material of the conveyor belt 11 is quartz, wherein SiO in the quartz2Is not less than 99.99%, whereby the above-mentioned conveyor belt 11 of quartz material is less likely to cause contamination of the polycrystalline silicon rod placed thereon at high temperature, thereby avoiding the problem of external contamination sources.
In the embodiment of the present invention, the material of the gear 12 is not particularly limited, and one skilled in the art may select the material at will according to actual needs as long as the gear 12 formed by the material is resistant to high temperature, and as a specific example, the material of the gear 12 is 304 stainless steel.
According to still other embodiments of the present invention, referring to fig. 2, the apparatus further includes a support 30, wherein the support 30 is disposed at the bottom of the heating chamber 20 and is connected to the side wall of the heating chamber 20 to support the heating chamber 20, and the lower surface of the bottom wall of the heating chamber 20 is suspended, so that the transfer unit 10 can rotate around the bottom wall of the heating chamber 20.
According to still other embodiments of the present invention, the door 21 is sealed with the opening 29 by the sealing layer 22, thereby further enhancing the sealing performance of the heating chamber 20 and preventing the silicon material from being oxidized in a high temperature environment. Further, the sealing layer 22 is made of teflon, so that the sealing layer 22 made of teflon has good sealing performance and high temperature resistance.
According to still other embodiments of the present invention, the heating chamber wall comprises two layers, an outer layer is made of 304 stainless steel, an inner layer is made of quartz, and SiO is contained in the quartz2The mass content of (A) is not less than 99.99%, therefore, the 304 stainless steel material has the characteristic of high temperature resistance, and the inner layer of the quartz material is not easy to cause pollution to the polycrystalline silicon rod at high temperature, thereby avoiding the problem of external pollution sources.
According to further embodiments of the present invention, a cooling water coil (not shown in the figures) is disposed between the outer layer and the inner layer, so that the body of the heating chamber 20 can be well protected even if the heating chamber 20 is heated too fast.
In an embodiment of the present invention, the electronic grade polysilicon thermal fragmentation heating apparatus further comprises a PCL control unit (not shown in the figure), and the PCL control unit is respectively connected to the heater 24 and the temperature detector 25, so that the temperature detector 25 feeds back the monitored temperature information in the heating chamber 20 to the PCL control unit, and the PCL control unit controls the heater 24 to perform automatic temperature control according to the temperature information.
Further, the heater 24 is a carbon fiber heating tube, which has the advantages of rapid temperature rise, small thermal lag, uniform heating, long thermal radiation transmission distance, high heat exchange speed and the like, and the luminous flux is far less than that of an electric heating tube of a metal heating body in the working process, and the electric heat conversion efficiency is up to more than 95%. Furthermore, the shell of the carbon fiber heating tube is made of SiO2The quartz with the mass content not less than 99.99 percent, and the quartz shell is not easy to cause pollution to the polysilicon rod at high temperature, thereby avoiding the problem of external pollution sources.
According to further embodiments of the present invention, a cylinder (not shown in the figures) is further disposed on the side wall of the heating chamber 20, and the cylinder is connected to the chamber door 21 through a connecting rod 23, so that the cylinder drives the chamber door 21 to open or close through the connecting rod 23.
According to still other embodiments of the present invention, a nano-filter 28 is disposed at the shielding gas inlet 27, and the purity of the shielding gas is further improved by filtering impurities in the shielding gas through the nano-filter 28. Further, the purity of the shielding gas entering the heating chamber 20 is not less than 99.999%, thereby further avoiding the problem of external pollution sources.
In the embodiment of the invention, the length of the polysilicon rod to be heated is 300-400mm, and the diameter is 150-250 mm.
In the embodiment of the present invention, the vacuum port 26 and the shielding gas inlet 27 are controlled by pneumatic control valves.
In the embodiment of the present invention, a plurality of heaters 24 are disposed on the inner wall of the heating chamber 20, and the plurality of heaters 24 are spaced apart from each other to uniformly heat the inside of the heating chamber 20.
In a second aspect of the invention, the invention provides a method for heating a polysilicon rod by using the electronic grade polysilicon thermal cracking heating device of the above embodiment. According to an embodiment of the invention, the method comprises:
(1) opening a bin gate 21, conveying the polycrystalline silicon rod to be heated to a heating bin 20 by using a conveying unit 10, and closing the bin gate 21 to enable the heating bin 20 to form a closed space;
in the step, an air cylinder is started, the air cylinder drives a bin gate 21 to be opened through a connecting rod, the polycrystalline silicon bar to be heated is conveyed into a heating bin 20 through a conveying unit 10, and the bin gate 21 is closed through the connecting rod driven by the air cylinder, so that the heating bin 20 forms a closed space.
(2) Evacuating the air in the heating chamber 20 through the vacuum-pumping port 26, and filling protective gas;
in this step, the air in the heating chamber 20 is evacuated through the vacuum-pumping port 26, and protective gas is filled to prevent the silicon material from being oxidized in a high-temperature environment. The specific kind of the above-mentioned shielding gas is not particularly limited, and as a specific example, the shielding gas may be nitrogen gas or inert gas.
(3) Starting the heater 24, and heating the polysilicon rod to 500-1000 ℃;
in the step, the heater 24 is started, the polysilicon rod is heated to 500-.
According to still other embodiments of the present invention, step (3) includes the following steps: starting a heater 24, and heating the polycrystalline silicon rod to 350-450 ℃ at a heating speed of 15-20 ℃/min; heating the polysilicon rod to 500-1000 ℃ at a heating speed of 25-35 ℃/min. Therefore, the materials in the bin body are uniformly heated by firstly heating to 450 ℃ at a lower heating speed and then heating to 1000 ℃ at a higher heating speed, and the preheating aims to ensure that the materials in the bin body are uniformly heated, so that the problem that the silicon materials are not uniformly heated due to too fast early heating is avoided, and the silicon material crushing size deviation is caused. Preferably, the polysilicon rod is heated to 400 ℃ at a heating rate of 20 ℃/min; and heating the polysilicon rod to 700 ℃ at a heating speed of 30 ℃/min.
(4) The bin gate 21 is opened, and the heated polysilicon rod is conveyed out of the heating bin 20 by the conveying unit 10.
In this step, after the polysilicon rod is heated, the air cylinder is started again, the air cylinder drives the bin gate 21 to open through the connecting rod, the heated polysilicon rod is conveyed out of the heating bin 20 through the conveying unit 10, and then the subsequent steps are performed.
According to the heating method of the embodiment of the invention, the polycrystalline silicon rod to be heated is conveyed into the heating bin 20 through the conveying unit 10, the bin door 21 is closed, the heating bin 20 forms a closed space, air in the heating bin 20 is evacuated through the vacuumizing port 26, and after the evacuation, protective gas is filled to block oxygen, so that the electronic-grade polycrystalline silicon rod is prevented from being oxidized due to high temperature in the heating process; starting the heater 24 to heat the polysilicon rod in the heating bin 20, and simultaneously monitoring the temperature in the heating bin 20 through the temperature detector 25; after the heating is completed, the gate 21 is opened, and the polycrystalline silicon rod after the heating is transferred out of the heating chamber 20 by the transfer unit 10. Therefore, the polycrystalline silicon rod automatically enters and exits the heating bin 20 through the conveying unit 10, and in the process of heating the polycrystalline silicon rod, other substances are not contacted except the conveying unit 10, and a single contact source is adopted, so that the problem of an external pollution source is avoided, and the heating efficiency is ensured.
In a third aspect of the invention, an electronic grade polysilicon thermal fragmentation device is presented. According to an embodiment of the present invention, the electronic grade polysilicon thermal fragmentation device has the electronic grade polysilicon thermal fragmentation heating device described in the above embodiment. Therefore, in the process that the polycrystalline silicon rod is heated in the electronic grade polycrystalline silicon thermal crushing device, other substances are not contacted except the conveying unit 10, and a single contact source is adopted, so that the problem of an external pollution source is avoided, and the heating efficiency is ensured.
In the embodiment of the invention, the electronic-grade polysilicon thermal-fragmentation heating device heats the silicon rod to be fragmented, and then the silicon rod is cooled and rapidly cooled, so that the polysilicon rod obtains an instant intercrystalline stress to be instantaneously fragmented.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. An electronic grade polysilicon thermal fragmentation heating device, comprising:
a transfer unit;
the heating chamber is provided with bin openings on two opposite side faces of the heating chamber, the conveying unit penetrates through the bin openings movably, bin doors are arranged at the bin openings, the heating chamber forms a closed space when the bin doors are closed, heaters and temperature detectors are arranged on the inner wall of the heating chamber, and vacuumizing ports and protective gas inlets are further formed in the wall of the heating chamber.
2. The electronic grade polysilicon thermal fragmentation heating apparatus of claim 1, wherein the conveyor unit comprises a gear and a conveyor belt, the conveyor belt being disposed on the gear, the upper surface of the bottom wall of the heating chamber being provided with a tooth mark corresponding to the gear.
3. The electronic grade polysilicon thermal fragmentation heating apparatus of claim 2, wherein the conveyor comprises a plurality of conveyor segments, a single conveyor segment having a length along the length of the conveyor unit of 8-12cm, and a distance between adjacent conveyor segments of 1.5-2.5 cm;
optionally, the material of the conveyor belt is quartz, and SiO in the quartz2The mass content of the gear is not less than 99.99 percent, and the material of the gear is 304 stainless steel.
4. The electronic grade polysilicon thermal fragmentation heating apparatus of claim 1, wherein the door is sealed to the port by a sealing layer;
optionally, the sealing layer is made of teflon.
5. The heating apparatus according to any one of claims 1 to 4, wherein the heating chamber wall comprises two layers, an outer layer is made of 304 stainless steel, an inner layer is made of quartz, and SiO is contained in the quartz2The mass content of the compound is not less than 99.99 percent;
optionally, a chilled water coil is disposed between the outer layer and the inner layer.
6. The electronic grade polysilicon thermal fragmentation heating apparatus of any of claims 1 to 4, wherein a cylinder is further provided on the side wall of the heating chamber, and the cylinder is connected to the chamber door by a connecting rod.
7. The electronic grade polysilicon thermal fragmentation heating apparatus of any of claims 1 to 4, wherein a nanofilter is provided at the shield gas inlet;
optionally, the purity of the shielding gas entering the heating chamber is not less than 99.999%.
8. The electronic grade polysilicon thermal fragmentation heating apparatus of any of claims 1 to 4, further comprising a PCL control unit connected to the heater and the temperature detector, respectively;
optionally, the heater is a carbon fiber heating tube.
9. A method of heating a polysilicon rod using the electronic grade polysilicon thermal fragmentation heating apparatus of any of claims 1 to 8, comprising:
(1) opening a bin door, conveying the polycrystalline silicon rod to be heated into a heating bin by adopting a conveying unit, and closing the bin door to form a closed space in the heating bin;
(2) evacuating air in the heating bin through a vacuumizing port, and filling protective gas;
(3) starting a heater, and heating the polysilicon rod to 500-1000 ℃;
(4) opening the bin door, and conveying the heated polycrystalline silicon rods out of the heating bin through the conveying unit;
optionally, step (3) comprises the steps of:
starting a heater, and heating the polysilicon rod to 350-450 ℃ at a heating speed of 15-20 ℃/min;
heating the polysilicon rod to 500-1000 ℃ at a heating speed of 25-35 ℃/min.
10. An electronic grade polysilicon thermal fragmentation device, wherein the electronic grade polysilicon thermal fragmentation device is provided with an electronic grade polysilicon thermal fragmentation heating device as claimed in any one of claims 1 to 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210135546.2A CN114534886A (en) | 2022-02-14 | 2022-02-14 | Electronic grade polycrystalline silicon thermal crushing heating device, heating method and crushing device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210135546.2A CN114534886A (en) | 2022-02-14 | 2022-02-14 | Electronic grade polycrystalline silicon thermal crushing heating device, heating method and crushing device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114534886A true CN114534886A (en) | 2022-05-27 |
Family
ID=81675643
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210135546.2A Pending CN114534886A (en) | 2022-02-14 | 2022-02-14 | Electronic grade polycrystalline silicon thermal crushing heating device, heating method and crushing device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114534886A (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102489372A (en) * | 2011-12-12 | 2012-06-13 | 湖南顶立科技有限公司 | Method and device for breaking polycrystalline silicon rod |
| CN202387534U (en) * | 2011-12-12 | 2012-08-22 | 湖南顶立科技有限公司 | Polysilicon rod crushing device |
| CN203053987U (en) * | 2013-01-22 | 2013-07-10 | 无锡研中科技有限公司 | Conveyor for test strips in reagent analyzer |
| CN203205389U (en) * | 2013-02-20 | 2013-09-18 | 富强半导体有限公司 | Heating furnace |
| CN110605176A (en) * | 2019-10-23 | 2019-12-24 | 西安华晶电子技术股份有限公司 | Method for breaking polycrystalline silicon material through water explosion |
| CN111001483A (en) * | 2019-12-31 | 2020-04-14 | 四川永祥多晶硅有限公司 | Polycrystalline silicon crushing system and polycrystalline silicon crushing method |
| CN111229421A (en) * | 2018-11-28 | 2020-06-05 | 江苏中能硅业科技发展有限公司 | Device and method for crushing polycrystalline silicon rod |
| CN212348852U (en) * | 2020-07-17 | 2021-01-15 | 自贡佳源炉业有限公司 | Material crushing system |
| CN213578759U (en) * | 2020-09-17 | 2021-06-29 | 江苏昌耐能源科技有限公司 | Heating furnace body with water-cooling jacket sleeve |
| CN215644408U (en) * | 2021-06-15 | 2022-01-25 | 江苏昌耐能源科技有限公司 | Heating furnace body with water-cooling shell and capable of achieving active jet flow rapid cooling |
-
2022
- 2022-02-14 CN CN202210135546.2A patent/CN114534886A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102489372A (en) * | 2011-12-12 | 2012-06-13 | 湖南顶立科技有限公司 | Method and device for breaking polycrystalline silicon rod |
| CN202387534U (en) * | 2011-12-12 | 2012-08-22 | 湖南顶立科技有限公司 | Polysilicon rod crushing device |
| CN203053987U (en) * | 2013-01-22 | 2013-07-10 | 无锡研中科技有限公司 | Conveyor for test strips in reagent analyzer |
| CN203205389U (en) * | 2013-02-20 | 2013-09-18 | 富强半导体有限公司 | Heating furnace |
| CN111229421A (en) * | 2018-11-28 | 2020-06-05 | 江苏中能硅业科技发展有限公司 | Device and method for crushing polycrystalline silicon rod |
| CN110605176A (en) * | 2019-10-23 | 2019-12-24 | 西安华晶电子技术股份有限公司 | Method for breaking polycrystalline silicon material through water explosion |
| CN111001483A (en) * | 2019-12-31 | 2020-04-14 | 四川永祥多晶硅有限公司 | Polycrystalline silicon crushing system and polycrystalline silicon crushing method |
| CN212348852U (en) * | 2020-07-17 | 2021-01-15 | 自贡佳源炉业有限公司 | Material crushing system |
| CN213578759U (en) * | 2020-09-17 | 2021-06-29 | 江苏昌耐能源科技有限公司 | Heating furnace body with water-cooling jacket sleeve |
| CN215644408U (en) * | 2021-06-15 | 2022-01-25 | 江苏昌耐能源科技有限公司 | Heating furnace body with water-cooling shell and capable of achieving active jet flow rapid cooling |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5857101B2 (en) | Method for determining the amount of impurities whose contaminants contribute to high purity silicon and furnace for processing high purity silicon | |
| KR101540225B1 (en) | Single Crystal Manufacturing Apparatus and Single Crystal Manufacturing Method | |
| CN107321977B (en) | Rare earth permanent magnet vacuum sintering method and vacuum sintering heat treatment equipment | |
| CN117466304B (en) | Silicon oxide production equipment | |
| CN102896391A (en) | Chain type vacuum furnace | |
| EP2149627B1 (en) | Quartz glass crucible for silicon single crystal pulling operation and process for manufacturing the same | |
| CN104016312B (en) | A kind of synthetic method of IIB-VIA compounds of group powder | |
| CN114534886A (en) | Electronic grade polycrystalline silicon thermal crushing heating device, heating method and crushing device | |
| KR101349263B1 (en) | Kiln with heating rollers | |
| CN113019301A (en) | Vertical quartz sand high-temperature chlorination device | |
| CN219752141U (en) | Quartz crucible preparation system | |
| KR101670453B1 (en) | Batch type apparatus for processing substrate | |
| JP3092267U (en) | Reactor with movable lid and aluminum nitride production equipment | |
| CN115573040A (en) | High-frequency coil heating annealing device for silicon rod and annealing method thereof | |
| CN115332147A (en) | High-temperature annealing furnace equipment | |
| CN205537094U (en) | Fill water cooling formula hydrogen sintering stove | |
| CN213514991U (en) | External heating type vacuum furnace | |
| CN112410732B (en) | In-situ pretreatment method for molecular beam epitaxy source material | |
| CN209188161U (en) | A kind of anhydrous rare earth halide purifying plant of high-quality | |
| TWI682077B (en) | Method for manufacturing silicon single crystal | |
| CN114345511A (en) | Thermal crushing method for electronic grade polycrystalline silicon rod | |
| CN114367371A (en) | Electronic grade polycrystalline silicon thermal crushing device | |
| CN103801700B (en) | RE permanent magnetic alloy flexibility hydrogen breaks process | |
| CN202804411U (en) | Chain type vacuum furnace | |
| CN117704802B (en) | Air pressure sintering furnace and operation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220527 |
|
| RJ01 | Rejection of invention patent application after publication |