CN101845667A - Method for producing high-resistivity monocrystalline silicon - Google Patents
Method for producing high-resistivity monocrystalline silicon Download PDFInfo
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- CN101845667A CN101845667A CN 201010213871 CN201010213871A CN101845667A CN 101845667 A CN101845667 A CN 101845667A CN 201010213871 CN201010213871 CN 201010213871 CN 201010213871 A CN201010213871 A CN 201010213871A CN 101845667 A CN101845667 A CN 101845667A
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Abstract
The invention discloses a method for producing high-resistivity monocrystalline silicon, comprising the following steps: melting and doping a polycrystalline silicon zone, purifying polycrystalline silicon in vacuum, and crystallizing a polycrystalline silicon rod. The method for producing the high-resistivity monocrystalline silicon can ensure that the monocrystalline silicon has the greatly improved purity of more than 10 N, the low cross-section resistivity heterogeneity nonuniformity of less than 15 percent, the long minority carrier lifetime of 1000 Mus and the high resistivity of more than 2000-7000 ohm.cm, thereby greatly improving the performance, the stability and the safety of the device and realizing the production of the high-resistivity monocrystalline silicon in the size by batch.
Description
Technical field
The present invention relates to a kind of preparation method of high-resistivity monocrystalline silicon.
Background technology
Zone melting technique is to utilize the grow method of single crystal of polycrystalline ingot subregion fusing and crystallization, it is seed crystal that this method is placed a fritter monocrystalline at the raw material head, and set up the melting zone in the seed crystal zone that links to each other with the raw material crystal ingot, mobile crystal ingot or well heater make the melting zone constantly move towards the crystal ingot length direction, crystallization again after the rest part of whole crystal ingot is melted successively, monocrystalline is constantly grown up.This technology can be used for production purity up to 99.999% semi-conductor, metal, alloy, inorganic and organic compound crystal.
The vacuum zone melting technology is to utilize the evaporation of impurity under the vacuum and the effect of segregation and a kind of method of obtaining the high purity silicon monocrystalline, under vacuum environment, purify and growing silicon single crystal, material is reached and keep higher purity, utilize this method can prepare the HIGH-PURITY SILICON monocrystalline of purity 11N.
The high purity silicon monocrystalline is to make various radiation detectors and the indispensable important materials of photodetector.But because the change of crystal growth condition, cause the volatilization of impurity and return making the very easily disconnected rib of monocrystalline, and make single crystal diameter be difficult to do greatly owing to lack atmosphere supporting power in the vacuum, so the vitellarium silicon crystal is more many than growing single-crystal difficulty in argon gas atmosphere in a vacuum.
In recent years, a lot of significant explorations and achievement in research have appearred in the technology for the preparation high-resistivity monocrystalline silicon:
As application number is the preparation method that 200910301603.4 patent application discloses a kind of vacuum zone melting high resistant silicon single crystal, but the disclosure patent is to be used for preparing resistivity to be (1-2) * 10
4The vacuum high resistance zone-melting silicon single-crystal of Ω cm, and the present invention prepares resistivity to be (2～7) * 10
3The vacuum high resistance zone-melting silicon single-crystal of Ω cm, this is the product of two kinds of different sizes, purposes is different.
Application number is the production method that 200610013497.6 patent application discloses a kind of vapor doping zone-melted silicon single crystal, but in the disclosure patent, the back polycrystalline that mixes is purified through vacuum, and product purity is low.
Existing preparation resistivity is (2～7) * 10
3The doping method of the vacuum high resistance zone-melting silicon single-crystal of Ω cm is a streak method, and the problem that this method exists is: doping agent is not easy to be evenly distributed in the crystal, and the radially resistivity distribution of different crystal there are differences, and the operation of configuration doping agent is cumbersome.The root of these problems is to use the unavoidable defective of this adulterating method, and personnel's individual difference and the doping of promptly mixing can't accurately be controlled and to cause.And the used adulterating method of this patent is the gas phase doping method, and impurity gas blows to the melting zone from nozzle, has increased the contact area in impurity gas and melting zone to a certain extent, helps axially and radial evenly mixes; In addition, in order further to improve adulterated homogeneity, we designed the doping hole in the melting zone in one week, thereby were more conducive to the reduction of ununiformity; And doping and doping time also can accurately be controlled by computer, have reached uniform doping, eliminate the purpose of individual difference and accurate controlled doping amount.
Summary of the invention
The objective of the invention is to:, provide a kind of preparation resistivity to be (2～7) * 10 at above problems of the prior art
3The production technique of the highly purified high resistance zone-melting silicon single-crystal of Ω cm.
In the production process of existing silicon single-crystal, had and added this processing step that mixes, the present invention is with existing adulterated difference: original gas doping technique is for just becoming brilliant under argon gas atmosphere after mixing, and the present invention combines gas phase doping with the vacuum zone melting technology, utilize the molten middle gas phase doping technology in atmosphere district that high-purity polycrystalline silicon raw material is mixed, increase useful foreign matter content wherein, and then purify by vacuum and to remove detrimental impurity and improve crystalline purity, under vacuum state, become brilliant at last.
In order to reach the foregoing invention purpose, the technical scheme that the invention process is following:
A kind of preparation method of high-resistivity monocrystalline silicon comprises that the molten doping of multi-crystal silicon area, vacuum are purified, the big technology of vacuum Cheng Jingsan, and its step is as follows:
(1) multi-crystal silicon area is molten mixes
A, prepurging, shove charge: clear up whole furnace chamber, adjust polycrystal, seed crystal, heater coil and go up center that axle, lower shaft make them point-blank;
B, bleed, inflation, preheating: open vacuum pump and pump-line valve, furnace chamber is vacuumized, vacuum tightness reaches 0.1Pa when following, closes pump-line valve and vacuum pump, charges into argon gas in burner hearth fast; After inflation finishes, polycrystalline silicon rod is carried out preheating;
C, change material, seeding: preheating is changed material after finishing; After the polycrystal fusing, seed crystal and molten silicon are carried out welding, seeding after the welding;
D, thin neck contracts: carry out the growth of thin neck, thin neck diameter 2-6mm, length 30-60mm;
E, open impurity gas: open the doping switch on the touch-screen, make impurity gas enter burner hearth, described impurity gas is the mixed gas of phosphine and argon gas or the mixed gas of borine and argon gas, and wherein phosphine, the shared concentration ratio of borine are 0.0001%-100%;
F, shouldering, commentaries on classics shoulder, isometrical: behind the thin neck growth ending, carry out shouldering, reduce moving down speed in the shouldering process to 1-8mm/min; When shouldering diameter and required crystal diameter differ 10-20mm, change shoulder, reach required diameter until crystal, change shoulder back isodiametric growth of crystal;
G, finish up, stop impurity gas, blowing out: when crystal is pulled to afterbody, begin to finish up and stop impurity gas, when the melting zone diameter is 10-20mm the melting zone is drawn back, last axle rises, and lower shaft descends;
(2) vacuum is purified
Polysilicon after mixing is purified under vacuum state, and preparation purity is the above high-purity polycrystalline silicon rod of 10N;
(3) vacuum Cheng Jing
With the high-purity polycrystalline silicon rod that above-mentioned steps obtains, under vacuum atmosphere, carry out silicon single crystal and become brilliant operation.
The object of the invention is further implemented by following optimal way:
As preferably, described vacuum purifying technique further comprises the steps:
(1) prepurging, shove charge operation:
Axle, lower shaft are pitched, gone up to a, the inwall with washed with de-ionized water vacuum zone melting single crystal growing furnace furnace chamber, heater coil, quartz, dry and extract indoor steam, detect dirt content, make the interior degree of cleaning of furnace chamber reach ten thousand grades, i.e. dust particle number≤10 of diameter more than 0.5 μ m
5/ m
3
B, seed crystal is installed on the seed crystal seat, attach it to the lower shaft top then;
C, will vertically be contained on the axle, and make the head of its lower end be in position above the center of horizontally disposed heater coil as the polycrystalline silicon rod after the doping of material; With the quartzy head that places on the heater coil and make the close polycrystalline silicon rod of its jaw level of pitching of the level of interior dress graphite; Close fire door, tighten each holding bolt;
(2) find time, preheating procedure:
D, startup mechanical pump vacuumize the vacuum zone melting single crystal growing furnace, and the vacuum tightness in furnace chamber reaches 10
-2During Pa, open molecular pump, the vacuum tightness in the furnace chamber is evacuated to 10
-3-10
-6Pa;
With the quartz fork polycrystalline silicon rod is carried out the indirec radiation preheating, be 20～30 minutes warm up time, treats to remove after polycrystalline silicon rod reddens quartzy fork, and the axle rotating speed is to 0.1-3rpm/min in the unlatching, and the lower shaft reverse speed makes the polycrystalline silicon rod thermally equivalent to 0.1-6rpm/min;
(3) change material, welding operation:
Preheating is changed material after finishing, and the lower shaft rotating speed is increased to 5～20rpm/min, carries out welding with moving the molten silicon that makes on seed crystal and the polycrystalline silicon rod on the lower shaft simultaneously;
(4) the thin neck operation of growth:
When seed crystal and polycrystalline silicon rod welding, upper and lower axle moved down simultaneously carry out thin neck process of growth, axle moves speed and is 1-2mm/min it on, and it is 5-20mm/min that lower shaft moves speed, and making thin neck grow to diameter is that 2～5mm, length are 40-60mm;
(5) shouldering operation: behind thin neck growth ending, carry out shouldering, promptly slowly reduce lower shaft and move speed to 1-5mm/min; Axle moves speed to 1-3mm/min in the change, makes head diameter slowly grow to equal diameter;
(6) change shoulder operation, isometrical and ending operation: when the aimed dia of shouldering diameter and this time polycrystalline silicon rod of purifying differed 5～8mm, shouldering speed is slowed to 2 ± 1mm/min changeed shoulder, until reaching required diameter; Keep isometrical process then, make it diameter and remain on 20～100mm, polycrystalline silicon growth speed is at 2～4mm/min; When polycrystalline silicon rod is pulled to afterbody, reduce heating power and finish up, reach 10～30mm to diameter, carry out purification next time again;
(7) repeat operation: press the quick travel button on the touch-screen, polycrystalline silicon rod is risen to polycrystal head shouldering position, flush with heater coil, repeat above-mentioned steps (3)-step (6) 2-20 time, is high-purity polycrystalline silicon rod more than the 10N thereby obtain purity.
As preferably, the described silicon single crystal that carries out under vacuum atmosphere becomes brilliant operation further to comprise the steps:
(1) prepurging, shove charge operation:
Axle, lower shaft are pitched, gone up to a, the inwall with washed with de-ionized water vacuum zone melting single crystal growing furnace furnace chamber, heater coil, quartz, dry and extract indoor steam, detect dirt content, make the interior degree of cleaning of furnace chamber reach ten thousand grades, i.e. dust particle number≤10 of diameter more than 0.5 μ m
5/ m
3
B, seed crystal is installed on the seed crystal seat, attach it to the lower shaft top then;
C, the purity that obtains of will purifying under vacuum atmosphere are that the high-purity polycrystalline silicon rod more than the 10N vertically is contained on the axle, make the head of its lower end be in position above the center of horizontally disposed heater coil; With the quartzy head that places on the heater coil and make the close polycrystalline silicon rod of its jaw level of pitching of the level of interior dress graphite;
D, close fire door, tighten each holding bolt;
(2) find time, preheating procedure:
E, startup mechanical pump vacuumize the vacuum zone melting single crystal growing furnace, and the vacuum tightness in furnace chamber reaches 10
-2During Pa, open molecular pump; Vacuum tightness in the furnace chamber is evacuated to 10
-3-10
-6Pa;
With the quartz fork polycrystalline silicon rod is carried out the indirec radiation preheating, be 20～30 minutes warm up time, treats to remove after polycrystalline silicon rod reddens quartzy fork, and the axle rotating speed is to 0.1-3rpm/min in the unlatching, and the lower shaft reverse speed makes the polycrystalline silicon rod thermally equivalent to 0.1-6rpm/min;
(3) change material, welding operation:
Preheating is changed material after finishing, and the lower shaft rotating speed is increased to 5～20rpm/min, carries out welding with moving the molten silicon that makes on seed crystal and the polycrystalline silicon rod on the lower shaft simultaneously;
(4) seeding operation: seed crystal and molten silicon are carried out welding, start after the welding and go up the lower shaft rotating speed, last axle rotating speed is to 1-2rpm/min, lower shaft rotating speed to 2～15rpm/min is adjusted lower shaft and is moved speed to 2～10mm/min, carries out thin neck growth, make thin neck diameter reach 2～5mm, length to 30～60mm;
(5) shouldering, commentaries on classics shoulder operation: behind thin neck growth ending, enter amplification process; Slowly reduce lower shaft and move speed to 2-4mm/min, and corresponding increase anode voltage is to 3-7KV, increase to go up the axle speed that moves down simultaneously and carry out the shouldering process to 5-8mm/min, when shouldering diameter and single crystal diameter differed 5～8mm, shouldering speed is slowed to 3～5mm/min changeed shoulder;
(6) isometrical, ending, blowing out operation: after changeing shoulder, carry out isodiametric growth with 2～4mm/min speed of growth; When being pulled to afterbody, silicon single crystal finishes up, reduction anode voltage and last axle move speed, dwindle diameter of silicon single crystal, when the melting zone diameter is 5～8mm, stop to go up axle and move speed, break the melting zone, keep lower shaft to move speed and rotating speed constant, receive point up to the melting zone, stop the radio-frequency generator power switch, stop lower shaft and move speed and rotating speed, stop molecular pump, mechanical pump; Promptly finally obtain required high-resistivity monocrystalline silicon product.
This patent adopts the order of mixing and afterwards purifying earlier, the benefit of doing like this is: when preparation N type monocrystalline, utilize the P content in the doping process increase crystal earlier, then by purify to adjust its content until crystal resistivity within target zone, and the detrimental impurity of removing simultaneously in the crystal improves crystalline purity; When preparation P type monocrystalline, repeatedly purify after the doping and can remove detrimental impurity and improve crystalline purity, and improve and mix impurity radially and vertical distributing homogeneity in crystal.
Adopt the inventive method to prepare silicon single-crystal, can greatly improve the purity of gained silicon single-crystal, obtain low section resistivity ununiformity and keep high minority carrier life time, monocrystalline resistivity reaches 2000 Ω .cm～7000 Ω .cm, its purity reaches more than the 10N, its section resistivity ununiformity is less than 15%, and minority carrier life time is greater than 1000 μ s, thereby greatly improves device performance and stability, security; Simultaneously can realize producing in batches the vacuum zone melting high resistant silicon single crystal of this specification.
Adopt the resistivity of four point probe resistivity tester specimen; Adopt minority carrier lifetime tester specimen minority carrier life time value; Detection to the silicon single-crystal sample defects is to use chemical corrosion method: carry out the corrosion of ASTM etching reagent again after earlier sample being handled through the CP-4 chemical brightening solution, adopt metallographic electron microscope observation sample defects then.The result shows, monocrystalline resistivity 2000 Ω cm-7000 Ω cm, and the life-span, the resistivity ununiformity was less than 15% greater than 1000 μ s, and microdefect is less than 100/cm
2Promptly there is not microdefect.
Embodiment
The preparation method of the high resistance zone-melting silicon single-crystal of embodiment 1 preparation Φ 40mm
Use the FZ-30 type zone melting single-crystal stove of rope company of Denmark Top production and the homemade vacuum zone melting single crystal growing furnace of QR-400 that the Beijing JingYunTong Science Co., Ltd produces, with the high-resistivity monocrystalline silicon of the inventive method production Φ 40mm, its quality reaches the SEMI standard.
The preparation method of this high-resistivity monocrystalline silicon comprises that in regular turn the molten doping of multi-crystal silicon area, vacuum purification become brilliant technology, operation as follows with vacuum:
1 multi-crystal silicon area is molten to mix
A, prepurging, shove charge: clear up whole furnace chamber, adjust polycrystal, seed crystal, heater coil and go up center that axle, lower shaft make them point-blank;
B, bleed, inflation, preheating: open vacuum pump and pump-line valve, furnace chamber is vacuumized, vacuum tightness reaches 0.1Pa when following, closes pump-line valve and vacuum pump, charges into argon gas in burner hearth fast; After inflation finishes, polycrystalline silicon rod is carried out preheating;
C, change material, seeding: preheating is changed material after finishing; After the polycrystal fusing, seed crystal and molten silicon are carried out welding, seeding after the welding;
D, thin neck contracts: carry out the growth of thin neck, thin neck diameter 2mm, length 30mm;
E, open impurity gas: open the doping switch on the touch-screen, make impurity gas enter burner hearth, described impurity gas is the mixed gas of phosphine and argon gas, wherein the shared concentration ratio of phosphine is 0.0001%;
F, shouldering, commentaries on classics shoulder, isometrical: behind the thin neck growth ending, carry out shouldering, reduce moving down speed in the shouldering process to 1mm/min; When shouldering diameter and required crystal diameter differ 10mm, change shoulder, reach required diameter until crystal, change shoulder back isodiametric growth of crystal;
G, finish up, stop impurity gas, blowing out: when crystal is pulled to afterbody, begin to finish up and stop impurity gas, when the melting zone diameter is 10mm the melting zone is drawn back, last axle rises, and lower shaft descends.
2 vacuum are purified
Polysilicon after mixing is purified under vacuum state, and preparation purity is the above high-purity polycrystalline silicon rod of 10N;
(1) prepurging, shove charge operation:
Axle, lower shaft are pitched, gone up to a, the inwall with washed with de-ionized water vacuum zone melting single crystal growing furnace furnace chamber, heater coil, quartz, dry and extract indoor steam, detect dirt content, make the interior degree of cleaning of furnace chamber reach ten thousand grades, i.e. dust particle number≤10 of diameter more than 0.5 μ m
5/ m
3
B, seed crystal is installed on the seed crystal seat, attach it to the lower shaft top then;
C, will vertically be contained on the axle, and make the head of its lower end be in position above the center of horizontally disposed heater coil as the polycrystalline silicon rod after the doping of material; With the quartzy head that places on the heater coil and make the close polycrystalline silicon rod of its jaw level of pitching of the level of interior dress graphite; Close fire door, tighten each holding bolt;
(2) find time, preheating procedure:
D, startup mechanical pump vacuumize the vacuum zone melting single crystal growing furnace, and the vacuum tightness in furnace chamber reaches 10
-2During Pa, open molecular pump, the vacuum tightness in the furnace chamber is evacuated to 10
-3Pa;
With the quartz fork polycrystalline silicon rod is carried out the indirec radiation preheating, be 20 minutes warm up time, treats to remove after polycrystalline silicon rod reddens quartzy fork, and the axle rotating speed is to 0.1rpm/min in the unlatching, and the lower shaft reverse speed makes the polycrystalline silicon rod thermally equivalent to 0.1rpm/min;
(3) change material, welding operation:
Preheating is changed material after finishing, and the lower shaft rotating speed is increased to 5rpm/min, carries out welding with moving the molten silicon that makes on seed crystal and the polycrystalline silicon rod on the lower shaft simultaneously;
(4) the thin neck operation of growth:
When seed crystal and polycrystalline silicon rod welding, upper and lower axle moved down simultaneously carry out thin neck process of growth, axle moves speed and is 1mm/min it on, and it is 5mm/min that lower shaft moves speed, and making thin neck grow to diameter is that 2mm, length are 40mm;
(5) shouldering operation: behind thin neck growth ending, carry out shouldering, promptly slowly reduce lower shaft and move speed to 1mm/min; Axle moves speed to 1mm/min in the change, makes head diameter slowly grow to equal diameter;
(6) change shoulder operation, isometrical and ending operation: when the aimed dia of shouldering diameter and this time polycrystalline silicon rod of purifying differed 5mm, shouldering speed is slowed to 2mm/min changeed shoulder, until reaching required diameter; Keep isometrical process then, make it diameter and remain on 20mm, polycrystalline silicon growth speed is at 2mm/min; When polycrystalline silicon rod is pulled to afterbody, reduce heating power and finish up, reach 10mm to diameter, carry out purification next time again.
(7) repeat operation: press the quick travel button on the touch-screen, polycrystalline silicon rod is risen to polycrystal head shouldering position, flush with heater coil, repeat above-mentioned steps (3)-step (6) 2 times, is high-purity polycrystalline silicon rod more than the 10N thereby obtain purity.
3, vacuum Cheng Jing
(1) prepurging, shove charge operation:
Axle, lower shaft are pitched, gone up to a, the inwall with washed with de-ionized water vacuum zone melting single crystal growing furnace furnace chamber, heater coil, quartz, dry and extract indoor steam, detect dirt content, make the interior degree of cleaning of furnace chamber reach ten thousand grades, i.e. dust particle number≤10 of diameter more than 0.5 μ m
5/ m
3
B, seed crystal is installed on the seed crystal seat, attach it to the lower shaft top then;
C, the purity that obtains of will purifying under vacuum atmosphere are that the high-purity polycrystalline silicon rod more than the 10N vertically is contained on the axle, make the head of its lower end be in position above the center of horizontally disposed heater coil; With the quartzy head that places on the heater coil and make the close polycrystalline silicon rod of its jaw level of pitching of the level of interior dress graphite;
D, close fire door, tighten each holding bolt;
(2) find time, preheating procedure:
E, startup mechanical pump vacuumize the vacuum zone melting single crystal growing furnace, and the vacuum tightness in furnace chamber reaches 10
-2During Pa, open molecular pump; Vacuum tightness in the furnace chamber is evacuated to 10
-3Pa;
With the quartz fork polycrystalline silicon rod is carried out the indirec radiation preheating, be 20 minutes warm up time, treats to remove after polycrystalline silicon rod reddens quartzy fork, and the axle rotating speed is to 0.1rpm/min in the unlatching, and the lower shaft reverse speed makes the polycrystalline silicon rod thermally equivalent to 0.1rpm/min;
(3) change material, welding operation:
Preheating is changed material after finishing, and the lower shaft rotating speed is increased to 5rpm/min, carries out welding with moving the molten silicon that makes on seed crystal and the polycrystalline silicon rod on the lower shaft simultaneously;
(4) seeding operation: seed crystal and molten silicon are carried out welding, start after the welding and go up the lower shaft rotating speed, last axle rotating speed is to 1rpm/min, and the lower shaft rotating speed is adjusted lower shaft and moved speed to 2mm/min to 2rpm/min, carries out thin neck growth, makes thin neck diameter reach 2mm, and length is to 30mm;
(5) shouldering, commentaries on classics shoulder operation: behind thin neck growth ending, enter amplification process; Slowly reduce lower shaft and move speed to 2mm/min, and corresponding increase anode voltage is to 3KV, increase simultaneously and go up the axle speed that moves down and carry out the shouldering process to 5mm/min, when shouldering diameter and single crystal diameter differed 5mm, shouldering speed is slowed to 3mm/min changeed shoulder;
(6) isometrical, ending, blowing out operation: after changeing shoulder, carry out isodiametric growth with the 2mm/min speed of growth; When being pulled to afterbody, silicon single crystal finishes up, reduction anode voltage and last axle move speed, dwindle diameter of silicon single crystal, stop to go up axle during for 5mm until the melting zone diameter and move speed, break the melting zone, keep lower shaft to move speed and rotating speed constant, receive point up to the melting zone, stop the radio-frequency generator power switch, stop lower shaft and move speed and rotating speed, stop molecular pump, mechanical pump; Promptly finally obtain required high-resistivity monocrystalline silicon product.
The preparation method of the high resistance zone-melting silicon single-crystal of embodiment 2 preparation Φ 45mm
Use the FZ-30 type zone melting single-crystal stove of rope company of Denmark Top production and the homemade vacuum zone melting single crystal growing furnace of QR-400 that the Beijing JingYunTong Science Co., Ltd produces, produce with the inventive method
Φ 45mmHigh-resistivity monocrystalline silicon, its quality reaches the SEMI standard.
The preparation method of this high-resistivity monocrystalline silicon comprises that in regular turn the molten doping of multi-crystal silicon area, vacuum purification become brilliant technology, operation as follows with vacuum:
1 multi-crystal silicon area is molten to mix
A, prepurging, shove charge: clear up whole furnace chamber, adjust polycrystal, seed crystal, heater coil and go up center that axle, lower shaft make them point-blank;
B, bleed, inflation, preheating: open vacuum pump and pump-line valve, furnace chamber is vacuumized, vacuum tightness reaches 0.1Pa when following, closes pump-line valve and vacuum pump, charges into argon gas in burner hearth fast; After inflation finishes, polycrystalline silicon rod is carried out preheating;
C, change material, seeding: preheating is changed material after finishing; After the polycrystal fusing, seed crystal and molten silicon are carried out welding, seeding after the welding;
D, thin neck contracts: carry out the growth of thin neck, thin neck diameter 6mm, length 60mm;
E, open impurity gas: open the doping switch on the touch-screen, make impurity gas enter burner hearth, described impurity gas is the mixed gas of borine and argon gas, and wherein the shared concentration ratio of borine is 0.0001%;
F, shouldering, commentaries on classics shoulder, isometrical: behind the thin neck growth ending, carry out shouldering, reduce moving down speed in the shouldering process to 8mm/min; When shouldering diameter and required crystal diameter differ 20mm, change shoulder, reach required diameter until crystal, change shoulder back isodiametric growth of crystal;
G, finish up, stop impurity gas, blowing out: when crystal is pulled to afterbody, begin to finish up and stop impurity gas, when the melting zone diameter is 20mm the melting zone is drawn back, last axle rises, and lower shaft descends.
2 vacuum are purified
Polysilicon after mixing is purified under vacuum state, and preparation purity is the above high-purity polycrystalline silicon rod of 10N;
(1) prepurging, shove charge operation:
Axle, lower shaft are pitched, gone up to a, the inwall with washed with de-ionized water vacuum zone melting single crystal growing furnace furnace chamber, heater coil, quartz, dry and extract indoor steam, detect dirt content, make the interior degree of cleaning of furnace chamber reach ten thousand grades, i.e. dust particle number≤10 of diameter more than 0.5 μ m
5/ m
3
B, seed crystal is installed on the seed crystal seat, attach it to the lower shaft top then;
C, will vertically be contained on the axle, and make the head of its lower end be in position above the center of horizontally disposed heater coil as the polycrystalline silicon rod after the doping of material; With the quartzy head that places on the heater coil and make the close polycrystalline silicon rod of its jaw level of pitching of the level of interior dress graphite; Close fire door, tighten each holding bolt;
(2) find time, preheating procedure:
D, startup mechanical pump vacuumize the vacuum zone melting single crystal growing furnace, and the vacuum tightness in furnace chamber reaches 10
-2During Pa, open molecular pump, the vacuum tightness in the furnace chamber is evacuated to 10
-6Pa;
With the quartz fork polycrystalline silicon rod is carried out the indirec radiation preheating, be 30 minutes warm up time, treats to remove after polycrystalline silicon rod reddens quartzy fork, and the axle rotating speed is to 3rpm/min in the unlatching, and the lower shaft reverse speed makes the polycrystalline silicon rod thermally equivalent to 6rpm/min;
(3) change material, welding operation:
Preheating is changed material after finishing, and the lower shaft rotating speed is increased to 20rpm/min, carries out welding with moving the molten silicon that makes on seed crystal and the polycrystalline silicon rod on the lower shaft simultaneously;
(4) the thin neck operation of growth:
When seed crystal and polycrystalline silicon rod welding, upper and lower axle moved down simultaneously carry out thin neck process of growth, axle moves speed and is 2mm/min it on, and it is 20mm/min that lower shaft moves speed, and making thin neck grow to diameter is that 5mm, length are 60mm;
(5) shouldering operation: behind thin neck growth ending, carry out shouldering, promptly slowly reduce lower shaft and move speed to 5mm/min; Axle moves speed to 3mm/min in the change, makes head diameter slowly grow to equal diameter;
(6) change shoulder operation, isometrical and ending operation: when the aimed dia of shouldering diameter and this time polycrystalline silicon rod of purifying differed 8mm, shouldering speed is slowed to 3mm/min changeed shoulder, until reaching required diameter; Keep isometrical process then, make it diameter and remain on 100mm, polycrystalline silicon growth speed is at 4mm/min; When polycrystalline silicon rod is pulled to afterbody, reduce heating power and finish up, reach 30mm to diameter, carry out purification next time again.
(7) repeat operation: press the quick travel button on the touch-screen, polycrystalline silicon rod is risen to polycrystal head shouldering position, flush with heater coil, repeat above-mentioned steps (3)-step (6) 20 times, is high-purity polycrystalline silicon rod more than the 10N thereby obtain purity.
3, vacuum Cheng Jing
(1) prepurging, shove charge operation:
Axle, lower shaft are pitched, gone up to a, the inwall with washed with de-ionized water vacuum zone melting single crystal growing furnace furnace chamber, heater coil, quartz, dry and extract indoor steam, detect dirt content, make the interior degree of cleaning of furnace chamber reach ten thousand grades, i.e. dust particle number≤10 of diameter more than 0.5 μ m
5/ m
3
B, seed crystal is installed on the seed crystal seat, attach it to the lower shaft top then;
C, the purity that obtains of will purifying under vacuum atmosphere are that the high-purity polycrystalline silicon rod more than the 10N vertically is contained on the axle, make the head of its lower end be in position above the center of horizontally disposed heater coil; With the quartzy head that places on the heater coil and make the close polycrystalline silicon rod of its jaw level of pitching of the level of interior dress graphite;
D, close fire door, tighten each holding bolt;
(2) find time, preheating procedure:
E, startup mechanical pump vacuumize the vacuum zone melting single crystal growing furnace, and the vacuum tightness in furnace chamber reaches 10
-2During Pa, open molecular pump; Vacuum tightness in the furnace chamber is evacuated to 10
-6Pa;
With the quartz fork polycrystalline silicon rod is carried out the indirec radiation preheating, be 30 minutes warm up time, treats to remove after polycrystalline silicon rod reddens quartzy fork, and the axle rotating speed is to 3rpm/min in the unlatching, and the lower shaft reverse speed makes the polycrystalline silicon rod thermally equivalent to 6rpm/min;
(3) change material, welding operation:
Preheating is changed material after finishing, and the lower shaft rotating speed is increased to 20rpm/min, carries out welding with moving the molten silicon that makes on seed crystal and the polycrystalline silicon rod on the lower shaft simultaneously;
(4) seeding operation: seed crystal and molten silicon are carried out welding, start after the welding and go up the lower shaft rotating speed, last axle rotating speed is to 2rpm/min, the lower shaft rotating speed is adjusted lower shaft and is moved speed to 10mm/min to 15rpm/min, carries out thin neck growth, make thin neck diameter reach 5mm, length is to 60mm;
(5) shouldering, commentaries on classics shoulder operation: behind thin neck growth ending, enter amplification process; Slowly reduce lower shaft and move speed to 4mm/min, and corresponding increase anode voltage is to 5KV, increase simultaneously and go up the axle speed that moves down and carry out the shouldering process to 8mm/min, when shouldering diameter and single crystal diameter differed 8mm, shouldering speed is slowed to 5mm/min changeed shoulder;
(6) isometrical, ending, blowing out operation: after changeing shoulder, carry out isodiametric growth with the 4mm/min speed of growth; When being pulled to afterbody, silicon single crystal finishes up, reduction anode voltage and last axle move speed, dwindle diameter of silicon single crystal, stop to go up axle during for 8mm until the melting zone diameter and move speed, break the melting zone, keep lower shaft to move speed and rotating speed constant, receive point up to the melting zone, stop the radio-frequency generator power switch, stop lower shaft and move speed and rotating speed, stop molecular pump, mechanical pump; Promptly finally obtain required high-resistivity monocrystalline silicon product
The preparation method of the vacuum zone melting high resistant silicon single crystal of embodiment 3 preparation Φ 50mm
Use the FZ-30 type zone melting single-crystal stove of rope company of Denmark Top production and the homemade vacuum zone melting single crystal growing furnace of QR-400 that the Beijing JingYunTong Science Co., Ltd produces, produce with the inventive method
Φ 50mmHigh-resistivity monocrystalline silicon, its quality reaches the SEMI standard.
The preparation method of this high-resistivity monocrystalline silicon comprises that in regular turn the molten doping of multi-crystal silicon area, vacuum purification become brilliant technology, operation as follows with vacuum:
1 multi-crystal silicon area is molten to mix
A, prepurging, shove charge: clear up whole furnace chamber, adjust polycrystal, seed crystal, heater coil and go up center that axle, lower shaft make them point-blank;
B, bleed, inflation, preheating: open vacuum pump and pump-line valve, furnace chamber is vacuumized, vacuum tightness reaches 0.1Pa when following, closes pump-line valve and vacuum pump, charges into argon gas in burner hearth fast; After inflation finishes, polycrystalline silicon rod is carried out preheating;
C, change material, seeding: preheating is changed material after finishing; After the polycrystal fusing, seed crystal and molten silicon are carried out welding, seeding after the welding;
D, thin neck contracts: carry out the growth of thin neck, thin neck diameter 4mm, length 45mm;
E, open impurity gas: open the doping switch on the touch-screen, make impurity gas enter burner hearth, described impurity gas is a phosphine;
F, shouldering, commentaries on classics shoulder, isometrical: behind the thin neck growth ending, carry out shouldering, reduce moving down speed in the shouldering process to 5mm/min; When shouldering diameter and required crystal diameter differ 15mm, change shoulder, reach required diameter until crystal, change shoulder back isodiametric growth of crystal;
G, finish up, stop impurity gas, blowing out: when crystal is pulled to afterbody, begin to finish up and stop impurity gas, when the melting zone diameter is 15mm the melting zone is drawn back, last axle rises, and lower shaft descends.
2 vacuum are purified
Polysilicon after mixing is purified under vacuum state, and preparation purity is the above high-purity polycrystalline silicon rod of 10N;
(1) prepurging, shove charge operation:
Axle, lower shaft are pitched, gone up to a, the inwall with washed with de-ionized water vacuum zone melting single crystal growing furnace furnace chamber, heater coil, quartz, dry and extract indoor steam, detect dirt content, make the interior degree of cleaning of furnace chamber reach ten thousand grades, i.e. dust particle number≤10 of diameter more than 0.5 μ m
5/ m
3
B, seed crystal is installed on the seed crystal seat, attach it to the lower shaft top then;
C, will vertically be contained on the axle, and make the head of its lower end be in position above the center of horizontally disposed heater coil as the polycrystalline silicon rod after the doping of material; With the quartzy head that places on the heater coil and make the close polycrystalline silicon rod of its jaw level of pitching of the level of interior dress graphite; Close fire door, tighten each holding bolt;
(2) find time, preheating procedure:
D, startup mechanical pump vacuumize the vacuum zone melting single crystal growing furnace, and the vacuum tightness in furnace chamber reaches 10
-2During Pa, open molecular pump, the vacuum tightness in the furnace chamber is evacuated to 10
-4Pa;
With the quartz fork polycrystalline silicon rod is carried out the indirec radiation preheating, be 25 minutes warm up time, treats to remove after polycrystalline silicon rod reddens quartzy fork, and the axle rotating speed is to 2rpm/min in the unlatching, and the lower shaft reverse speed makes the polycrystalline silicon rod thermally equivalent to 3rpm/min;
(3) change material, welding operation:
Preheating is changed material after finishing, and the lower shaft rotating speed is increased to 12rpm/min, carries out welding with moving the molten silicon that makes on seed crystal and the polycrystalline silicon rod on the lower shaft simultaneously;
(4) the thin neck operation of growth:
When seed crystal and polycrystalline silicon rod welding, upper and lower axle moved down simultaneously carry out thin neck process of growth, axle moves speed and is 1.5mm/min it on, and it is 12mm/min that lower shaft moves speed, and making thin neck grow to diameter is that 3mm, length are 50mm;
(5) shouldering operation: behind thin neck growth ending, carry out shouldering, promptly slowly reduce lower shaft and move speed to 3mm/min; Axle moves speed to 2mm/min in the change, makes head diameter slowly grow to equal diameter;
(6) change shoulder operation, isometrical and ending operation: when the aimed dia of shouldering diameter and this time polycrystalline silicon rod of purifying differed 6mm, shouldering speed is slowed to 1mm/min changeed shoulder, until reaching required diameter; Keep isometrical process then, make it diameter and remain on 60mm, polycrystalline silicon growth speed is at 3mm/min; When polycrystalline silicon rod is pulled to afterbody, reduce heating power and finish up, reach 20mm to diameter, carry out purification next time again.
(7) repeat operation: press the quick travel button on the touch-screen, polycrystalline silicon rod is risen to polycrystal head shouldering position, flush with heater coil, repeat above-mentioned steps (3)-step (6) 12 times, is high-purity polycrystalline silicon rod more than the 10N thereby obtain purity.
3, vacuum Cheng Jing
(1) prepurging, shove charge operation:
Axle, lower shaft are pitched, gone up to a, the inwall with washed with de-ionized water vacuum zone melting single crystal growing furnace furnace chamber, heater coil, quartz, dry and extract indoor steam, detect dirt content, make the interior degree of cleaning of furnace chamber reach ten thousand grades, i.e. dust particle number≤10 of diameter more than 0.5 μ m
5/ m
3
B, seed crystal is installed on the seed crystal seat, attach it to the lower shaft top then;
C, the purity that obtains of will purifying under vacuum atmosphere are that the high-purity polycrystalline silicon rod more than the 10N vertically is contained on the axle, make the head of its lower end be in position above the center of horizontally disposed heater coil; With the quartzy head that places on the heater coil and make the close polycrystalline silicon rod of its jaw level of pitching of the level of interior dress graphite;
D, close fire door, tighten each holding bolt;
(2) find time, preheating procedure:
E, startup mechanical pump vacuumize the vacuum zone melting single crystal growing furnace, and the vacuum tightness in furnace chamber reaches 10
-2During Pa, open molecular pump; Vacuum tightness in the furnace chamber is evacuated to 10
-4Pa;
With the quartz fork polycrystalline silicon rod is carried out the indirec radiation preheating, be 25 minutes warm up time, treats to remove after polycrystalline silicon rod reddens quartzy fork, and the axle rotating speed is to 2rpm/min in the unlatching, and the lower shaft reverse speed makes the polycrystalline silicon rod thermally equivalent to 3rpm/min;
(3) change material, welding operation:
Preheating is changed material after finishing, and the lower shaft rotating speed is increased to 12rpm/min, carries out welding with moving the molten silicon that makes on seed crystal and the polycrystalline silicon rod on the lower shaft simultaneously;
(4) seeding operation: seed crystal and molten silicon are carried out welding, start after the welding and go up the lower shaft rotating speed, last axle rotating speed is to 1.5rpm/min, the lower shaft rotating speed is adjusted lower shaft and is moved speed to 6mm/min to 8rpm/min, carries out thin neck growth, make thin neck diameter reach 4mm, length is to 45mm;
(5) shouldering, commentaries on classics shoulder operation: behind thin neck growth ending, enter amplification process; Slowly reduce lower shaft and move speed to 3mm/min, and corresponding increase anode voltage is to 7KV, increase simultaneously and go up the axle speed that moves down and carry out the shouldering process to 6mm/min, when shouldering diameter and single crystal diameter differed 6mm, shouldering speed is slowed to 4mm/min changeed shoulder;
(6) isometrical, ending, blowing out operation: after changeing shoulder, carry out isodiametric growth with the 3mm/min speed of growth; When being pulled to afterbody, silicon single crystal finishes up, reduction anode voltage and last axle move speed, dwindle diameter of silicon single crystal, stop to go up axle during for 6mm until the melting zone diameter and move speed, break the melting zone, keep lower shaft to move speed and rotating speed constant, receive point up to the melting zone, stop the radio-frequency generator power switch, stop lower shaft and move speed and rotating speed, stop molecular pump, mechanical pump; Promptly finally obtain required high-resistivity monocrystalline silicon product.
Claims (3)
1. the preparation method of a high-resistivity monocrystalline silicon comprises that the molten doping of multi-crystal silicon area, vacuum are purified, the big technology of vacuum Cheng Jingsan, and its step is as follows:
(1) multi-crystal silicon area is molten mixes
A, prepurging, shove charge: clear up whole furnace chamber, adjust polycrystal, seed crystal, heater coil and go up center that axle, lower shaft make them point-blank;
B, bleed, inflation, preheating: open vacuum pump and pump-line valve, furnace chamber is vacuumized, vacuum tightness reaches 0.1Pa when following, closes pump-line valve and vacuum pump, charges into argon gas in burner hearth fast; After inflation finishes, polycrystalline silicon rod is carried out preheating;
C, change material, seeding: preheating is changed material after finishing; After the polycrystal fusing, seed crystal and molten silicon are carried out welding, seeding after the welding;
D, thin neck contracts: carry out the growth of thin neck, thin neck diameter 2-6mm, length 30-60mm;
E, open impurity gas: open the doping switch on the touch-screen, make impurity gas enter burner hearth, described impurity gas is the mixed gas of phosphine and argon gas or the mixed gas of borine and argon gas, and wherein phosphine, the shared concentration ratio of borine are 0.0001%-100%;
F, shouldering, commentaries on classics shoulder, isometrical: behind the thin neck growth ending, carry out shouldering, reduce moving down speed in the shouldering process to 1-8mm/min; When shouldering diameter and required crystal diameter differ 10-20mm, change shoulder, reach required diameter until crystal, change shoulder back isodiametric growth of crystal;
G, finish up, stop impurity gas, blowing out: when crystal is pulled to afterbody, begin to finish up and stop impurity gas, when the melting zone diameter is 10-20mm the melting zone is drawn back, last axle rises, and lower shaft descends;
(2) vacuum is purified
Polysilicon after mixing is purified under vacuum state, and preparation purity is the above high-purity polycrystalline silicon rod of 10N;
(3) vacuum Cheng Jing
With the high-purity polycrystalline silicon rod that above-mentioned steps obtains, under vacuum atmosphere, carry out silicon single crystal and become brilliant operation.
2. the preparation method of high-resistivity monocrystalline silicon according to claim 1, it is characterized in that: described vacuum purifying technique further comprises the steps:
(1) prepurging, shove charge operation:
Axle, lower shaft are pitched, gone up to a, the inwall with washed with de-ionized water vacuum zone melting single crystal growing furnace furnace chamber, heater coil, quartz, dry and extract indoor steam, detect dirt content, make the interior degree of cleaning of furnace chamber reach ten thousand grades, i.e. dust particle number≤10 of diameter more than 0.5 μ m
5/ m
3
B, seed crystal is installed on the seed crystal seat, attach it to the lower shaft top then;
C, will vertically be contained on the axle, and make the head of its lower end be in position above the center of horizontally disposed heater coil as the polycrystalline silicon rod after the doping of material; With the quartzy head that places on the heater coil and make the close polycrystalline silicon rod of its jaw level of pitching of the level of interior dress graphite; Close fire door, tighten each holding bolt;
(2) find time, preheating procedure:
D, startup mechanical pump vacuumize the vacuum zone melting single crystal growing furnace, and the vacuum tightness in furnace chamber reaches 10
-2During Pa, open molecular pump, the vacuum tightness in the furnace chamber is evacuated to 10
-3-10
-6Pa;
With the quartz fork polycrystalline silicon rod is carried out the indirec radiation preheating, be 20～30 minutes warm up time, treats to remove after polycrystalline silicon rod reddens quartzy fork, and the axle rotating speed is to 0.1-3rpm/min in the unlatching, and the lower shaft reverse speed makes the polycrystalline silicon rod thermally equivalent to 0.1-6rpm/min;
(3) change material, welding operation:
Preheating is changed material after finishing, and the lower shaft rotating speed is increased to 5～20rpm/min, carries out welding with moving the molten silicon that makes on seed crystal and the polycrystalline silicon rod on the lower shaft simultaneously;
(4) the thin neck operation of growth:
When seed crystal and polycrystalline silicon rod welding, upper and lower axle moved down simultaneously carry out thin neck process of growth, axle moves speed and is 1-2mm/min it on, and it is 5-20mm/min that lower shaft moves speed, and making thin neck grow to diameter is that 2～5mm, length are 40-60mm;
(5) shouldering operation: behind thin neck growth ending, carry out shouldering, promptly slowly reduce lower shaft and move speed to 1-5mm/min; Axle moves speed to 1-3mm/min in the change, makes head diameter slowly grow to equal diameter;
(6) change shoulder operation, isometrical and ending operation: when the aimed dia of shouldering diameter and this time polycrystalline silicon rod of purifying differed 5～8mm, shouldering speed is slowed to 2 ± 1mm/min changeed shoulder, until reaching required diameter; Keep isometrical process then, make it diameter and remain on 20～100mm, polycrystalline silicon growth speed is at 2～4mm/min; When polycrystalline silicon rod is pulled to afterbody, reduce heating power and finish up, reach 10～30mm to diameter, carry out purification next time again;
(7) repeat operation: press the quick travel button on the touch-screen, polycrystalline silicon rod is risen to polycrystal head shouldering position, flush with heater coil, repeat above-mentioned steps (3)-step (6) 2-20 time, is high-purity polycrystalline silicon rod more than the 10N thereby obtain purity.
3. the preparation method of high-resistivity monocrystalline silicon according to claim 1 and 2, it is characterized in that: described vacuum becomes brilliant operation further to comprise the steps:
(1) prepurging, shove charge operation:
Axle, lower shaft are pitched, gone up to a, the inwall with washed with de-ionized water vacuum zone melting single crystal growing furnace furnace chamber, heater coil, quartz, dry and extract indoor steam, detect dirt content, make the interior degree of cleaning of furnace chamber reach ten thousand grades, i.e. dust particle number≤10 of diameter more than 0.5 μ m
5/ m
3
B, seed crystal is installed on the seed crystal seat, attach it to the lower shaft top then;
C, will be that high-purity polycrystalline silicon rod more than the 10N vertically is contained on the axle in the purity that obtains of purifying under the vacuum atmosphere in the step (2) of claim 1, make the head of its lower end be in position above the center of horizontally disposed heater coil; With the quartzy head that places on the heater coil and make the close polycrystalline silicon rod of its jaw level of pitching of the level of interior dress graphite;
D, close fire door, tighten each holding bolt;
(2) find time, preheating procedure:
E, startup mechanical pump vacuumize the vacuum zone melting single crystal growing furnace, and the vacuum tightness in furnace chamber reaches 10
-2During Pa, open molecular pump; Vacuum tightness in the furnace chamber is evacuated to 10
-3-10
-6Pa;
With the quartz fork polycrystalline silicon rod is carried out the indirec radiation preheating, be 20～30 minutes warm up time, treats to remove after polycrystalline silicon rod reddens quartzy fork, and the axle rotating speed is to 0.1-3rpm/min in the unlatching, and the lower shaft reverse speed makes the polycrystalline silicon rod thermally equivalent to 0.1-6rpm/min;
(3) change material, welding operation:
Preheating is changed material after finishing, and the lower shaft rotating speed is increased to 5～20rpm/min, carries out welding with moving the molten silicon that makes on seed crystal and the polycrystalline silicon rod on the lower shaft simultaneously;
(4) seeding operation: seed crystal and molten silicon are carried out welding, start after the welding and go up the lower shaft rotating speed, last axle rotating speed is to 1-2rpm/min, lower shaft rotating speed to 2～15rpm/min is adjusted lower shaft and is moved speed to 2～10mm/min, carries out thin neck growth, make thin neck diameter reach 2～5mm, length to 30～60mm;
(5) shouldering, commentaries on classics shoulder operation: behind thin neck growth ending, enter amplification process; Slowly reduce lower shaft and move speed to 2-4mm/min, and corresponding increase anode voltage is to 3-7KV, increase to go up the axle speed that moves down simultaneously and carry out the shouldering process to 5-8mm/min, when shouldering diameter and single crystal diameter differed 5～8mm, shouldering speed is slowed to 3～5mm/min changeed shoulder;
(6) isometrical, ending, blowing out operation: after changeing shoulder, carry out isodiametric growth with 2～4mm/min speed of growth; When being pulled to afterbody, silicon single crystal finishes up, reduction anode voltage and last axle move speed, dwindle diameter of silicon single crystal, when the melting zone diameter is 5～8mm, stop to go up axle and move speed, break the melting zone, keep lower shaft to move speed and rotating speed constant, receive point up to the melting zone, stop the radio-frequency generator power switch, stop lower shaft and move speed and rotating speed, stop molecular pump, mechanical pump; Promptly finally obtain required high-resistivity monocrystalline silicon product.
?
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| CN101979719A (en) * | 2010-11-03 | 2011-02-23 | 天津市环欧半导体材料技术有限公司 | Method for producing gas phase heavy phosphorus-doped float zone silicon single crystal |
| CN102534750A (en) * | 2012-03-08 | 2012-07-04 | 天津市环欧半导体材料技术有限公司 | Traveling wave magnetic field method for improving resistivity uniformity of zone-melted silicon single crystal |
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| CN106702473B (en) * | 2015-07-20 | 2019-05-21 | 有研半导体材料有限公司 | Prevention polycrystalline goes out the technique pierced in a kind of growth of zone-melted silicon single crystal |
| CN106498495B (en) * | 2016-11-02 | 2018-09-11 | 中国电子科技集团公司第四十六研究所 | A kind of process for surface preparation of vacuum zone-melting silicon monocrystal growth heating coil |
| CN106498495A (en) * | 2016-11-02 | 2017-03-15 | 中国电子科技集团公司第四十六研究所 | A kind of process for surface preparation of vacuum zone-melting silicon monocrystal growth heating coil |
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| CN106370931B (en) * | 2016-11-14 | 2023-06-23 | 山东辰宇稀有材料科技有限公司 | Silicon material batching and segregation device and method |
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