CN103422156A - Production method of technique of one-step crystallization of polycrystalline silicon material in FZ monocrystalline silicon - Google Patents
Production method of technique of one-step crystallization of polycrystalline silicon material in FZ monocrystalline silicon Download PDFInfo
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- CN103422156A CN103422156A CN2012101633002A CN201210163300A CN103422156A CN 103422156 A CN103422156 A CN 103422156A CN 2012101633002 A CN2012101633002 A CN 2012101633002A CN 201210163300 A CN201210163300 A CN 201210163300A CN 103422156 A CN103422156 A CN 103422156A
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Abstract
The invention relates to a production method of a technique of one-step crystallization of polycrystalline silicon material in FZ monocrystalline silicon. The method comprises the following steps: obtaining polycrystalline silicon through cleaning with a ultrasonic cleaner; transferring the polycrystalline silicon into a zone-melting single-crystal furnace; melting and connecting a seed crystal with molten silicon; after the melting and connecting, starting to increase the rotation speeds of an upper shaft and a lower shaft; and after a necking process, carrying out crowning, bubble removal, and shoulder-extending processing, as well as equal-diameter growth, tail formation, and furnace shutdown processes. The method has the following beneficial effects: by means of the technique, consumption of various energy is lowered during production process, the utilization rate of environment is improved, and the crystallization technique is simplified relatively; operation state of the FZ monocrystalline silicon crystallization technique can be changed, and monocrystalline silicon products are increased in yield rate and decreased in defective rate, so that costs are reduced; the changed FZ monocrystalline silicon technique can also reduce the cost of the polycrystalline silicon material and the number of times of head and tail formation; and loss of the polycrystalline silicon material caused by pollution of impurities generated during purification of the polycrystalline silicon material can be reduced.
Description
Technical field
The present invention relates to the zone-melted silicon single crystal growth technique, relate in particular to the brilliant its preparation process of the once one-tenth of a kind of polycrystal in study on floating zone silicon.
Background technology
For monocrystalline growing process, adopt the floating zone melting principle of work to be: melting zone is suspended state, with any material, does not contact, thereby can not be stain, and the effect of segregation and evaporative effect due to impurity in silicon, can obtain the HIGH-PURITY SILICON monocrystalline.District is molten can carry out in protective atmosphere (argon, hydrogen), also can carry out in a vacuum, and can repeatedly purify, and is particularly useful for making high-resistivity monocrystalline silicon and detector grade HIGH-PURITY SILICON monocrystalline; When drawing, utilize copper coil by the local thawing of the material of polysilicon pole, by the ring-band shape well heater, to produce the local phenomenon of melting, control again process of setting and the growing single-crystal rod, when growing single-crystal, make cylindrical silicon rod be fixed in the vertical direction rotation, with radio-frequency induction coil, in argon gas atmosphere, heat, make excellent bottom and form molten drop in its underpart between close co-axially fixed single crystal seed, these two rods rotate in the opposite direction, the melting zone that then will between polycrystalline rod and seed crystal, only depend on surface tension to form progressively moves up along rod is long, converts thereof into monocrystalline.Current common one-tenth crystal type is sequentially that polycrystalline silicon purifying becomes brilliant two large techniques with silicon single-crystal, and wherein, polycrystalline silicon purifying comprises prepurging, shove charge, finds time, preheating, material, welding, the thin neck of growth, shouldering, turn shoulder, isometrical and finish up, repetition; Wherein, silicon single crystal Cheng Jing comprises prepurging, shove charge, finds time, preheating, material processing, seeding, shouldering, turns shoulder operation, isometrical, ending, blowing out.But, for current method, the loss of the various energy is larger, from forming brilliant technique, also simplify not.Therefore, for above aspect, need to be upgraded prior art.
Summary of the invention
For above defect, the invention provides the brilliant its preparation process of the once one-tenth of a kind of polycrystal in study on floating zone silicon, thereby can solve the contaminating impurity brought because of in the polycrystal raw material purification process, reduced simultaneously the various energy loss, saved the environment utilization ratio, become brilliant technique relatively to oversimplify.
For achieving the above object, the present invention is by the following technical solutions:
The brilliant its preparation process of the once one-tenth of a kind of polycrystal in study on floating zone silicon, realize in accordance with the following steps:
(1) raw material to be processed is cut off, cutting;
(2) surface particles is removed to the clean extremely smooth brightness that has, re-used Ultrasonic Cleaners and clean the corrosion raw material, add the allocation processing agent simultaneously after cleaning, again clean the polysilicon that obtains having relatively high expectations;
(3) by the polysilicon of above-mentioned processing, proceed in the zone melting single-crystal stove that shielding gas exists, then carry out prepurging, shove charge, find time, preheating, material treatment step;
(4) seed crystal and molten silicon are carried out to welding, start upper lower shaft rotating speed after welding, upper axle rotating speed to 1～2rpm/min, lower shaft rotating speed to 2～15rpm/min, adjust lower shaft and move speed to 2～14mm/min, carries out thin neck growth, make thin neck diameter reach 3～5mm, length reaches 60～90mm;
(5), after thin neck is grown end, carry out shouldering, go out bag, expand the shoulder processing; Slowly reduce lower shaft and move speed to 3～5mm/min, and corresponding increase current/voltage to 4～7kv, the upper axle of increase simultaneously moves down speed to 6～8mm/min and carries out the shouldering process, when shouldering diameter and single crystal diameter differ 5～10mm, shouldering speed is slowed to 3～4mm/min and turned shoulder, make it to reach silicon single crystal aimed dia 51～55mm;
(6) when reaching the silicon single crystal aimed dia, with 2～4 ± 1mm/min speed of growth, carry out isodiametric growth, and running status when simultaneously starting to rotate and reverse; When silicon single crystal is pulled to afterbody and is finished up, the state that stops rotating speed becoming a single state and the operation of equidirectional state, slowly reduces power and upper axle moves speed, dwindles diameter of silicon single crystal, until differ 5～10mm with required finished product single crystal diameter, move speed on going up axially, break melting zone, the maintenance lower shaft moves speed and rotating speed is not changed direction constant, until the melting zone epilog completes, high pressure is in maintaining condition, and blowing out cooling time is 1 hour, carries out the product that the prepurging operation can obtain zone-melted silicon single crystal.
The beneficial effect that once become brilliant its preparation process of polycrystal of the present invention in study on floating zone silicon is: the zone melting method silicon single-crystal of producing can reach resistivity, ultrapurity, resistivity distribution, the section resistivity evenness with the rear one-tenth crystal silicon monocrystalline that equals to purify, more than its purity reaches 11N, resistivity reaches N-type>1500 Ω .cm, the section resistivity evenness is less than 15%, thereby greatly improves device performance; Utilize this technique, can reduce in process of production the loss of the various energy, save the environment utilization ratio, make into brilliant technique and relatively oversimplify; Can change the running status that zone-melted silicon single crystal becomes brilliant technique, improve the quality of silicon single-crystal, for the implementation process of adulterating, improve silicon single-crystal finished product rate, reduce and a grade rate, relatively save cost; By the zone-melted silicon single crystal technique changed, aspect the raw material polysilicon also cost-saved, reduce end to end number of times, reduce material loss; Can relatively solve the contaminating impurity brought because of in the polycrystal raw material purification process from becoming crystalline substance, cause unnecessary material loss.
Embodiment
The brilliant its preparation process of the once one-tenth of the described polycrystal of the embodiment of the present invention in study on floating zone silicon, comprise the steps:
(1) blank: by raw material to be processed cut off, cutting;
(2) polycrystal raw material is polished, is cleaned: by the clean extremely smooth brightness that has of surface particles removal, re-use Ultrasonic Cleaners cleaning corrosion raw material, avoid affecting into crystalline substance, add the allocation processing agent simultaneously after cleaning, again cleaning; Until make every mass parameter of polycrystalline silicon rod meet every mass parameter requirement of producing study on floating zone silicon, then obtain the polysilicon of having relatively high expectations;
(3) silicon single crystal becomes brilliant operation: by the polysilicon of above-mentioned processing, proceed in the zone melting single-crystal stove that shielding gas exists, then carry out prepurging, shove charge, find time, preheating, material treatment step;
(4) seeding operation: seed crystal and molten silicon are carried out to welding, start upper lower shaft rotating speed after welding, upper axle rotating speed to 1～2rpm/min, lower shaft rotating speed to 2～15rpm/min, adjust lower shaft and move speed to 2～14mm/min, carries out thin neck growth, make thin neck diameter reach 3～5mm, length to 60～90mm;
(5) shouldering, turn the shoulder operation: after thin neck growth finishes, carry out shouldering, go out bag, expand shoulder and process; Slowly reduce lower shaft and move speed to 4 ± 1mm/min, and corresponding increase current/voltage to 4～7kv, the upper axle of increase simultaneously moves down speed to 6～8mm/min and carries out the shouldering process, when shouldering diameter and single crystal diameter differ 5～10mm, shouldering speed is slowed to 3～4mm/min and turned shoulder, make it to reach silicon single crystal aimed dia 53 ± 2mm;
(6) isometrical, ending, blowing out operation: when reaching the silicon single crystal aimed dia, with 2～4 ± 1mm/min speed of growth, carry out isodiametric growth, and running status when simultaneously starting to rotate and reverse; When silicon single crystal is pulled to afterbody and is finished up, the state that stops rotating speed becoming a single state and the operation of equidirectional state, slowly reduces power and upper axle moves speed, dwindles diameter of silicon single crystal, until differ 5～10mm with required finished product single crystal diameter, move speed on going up axially, break melting zone, the maintenance lower shaft moves speed and rotating speed is not changed direction constant, until the melting zone epilog completes, high pressure is in maintaining condition, and blowing out cooling time is 1 hour, carries out the product that the prepurging operation can obtain zone-melted silicon single crystal.
Above embodiment is more preferably embodiment a kind of of the present invention, the common variation that those skilled in the art carry out in the technical program scope and replace and should be included in protection scope of the present invention.
Claims (1)
1. the brilliant its preparation process of the once one-tenth of a polycrystal in study on floating zone silicon, is characterized in that, realizes in accordance with the following steps:
(1) raw material to be processed is cut off, cutting;
(2) surface particles is removed to the clean extremely smooth brightness that has, re-used Ultrasonic Cleaners and clean the corrosion raw material, add the allocation processing agent simultaneously after cleaning, again clean the polysilicon that obtains having relatively high expectations;
(3) by the polysilicon of above-mentioned processing, proceed in the zone melting single-crystal stove that shielding gas exists, then carry out prepurging, shove charge, find time, preheating, material treatment step;
(4) seed crystal and molten silicon are carried out to welding, start upper lower shaft rotating speed after welding, upper axle rotating speed to 1～2rpm/min, lower shaft rotating speed to 2～15rpm/min, adjust lower shaft and move speed to 2～14mm/min, carries out thin neck growth, make thin neck diameter reach 3～5mm, length reaches 60～90mm;
(5), after thin neck is grown end, carry out shouldering, go out bag, expand the shoulder processing; Slowly reduce lower shaft and move speed to 3～5mm/min, and corresponding increase current/voltage to 4～7kv, the upper axle of increase simultaneously moves down speed to 6～8mm/min and carries out the shouldering process, when shouldering diameter and single crystal diameter differ 5～10mm, shouldering speed is slowed to 3～4mm/min and turned shoulder, make it to reach silicon single crystal aimed dia 51～55mm;
(6) when reaching the silicon single crystal aimed dia, with 2～4 ± 1mm/min speed of growth, carry out isodiametric growth, and running status when simultaneously starting to rotate and reverse; When silicon single crystal is pulled to afterbody and is finished up, the state that stops rotating speed becoming a single state and the operation of equidirectional state, slowly reduces power and upper axle moves speed, dwindles diameter of silicon single crystal, until differ 5～10mm with required finished product single crystal diameter, move speed on going up axially, break melting zone, the maintenance lower shaft moves speed and rotating speed is not changed direction constant, until the melting zone epilog completes, high pressure is in maintaining condition, and blowing out cooling time is 1 hour, carries out the product that the prepurging operation can obtain zone-melted silicon single crystal.
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| CN106222745A (en) * | 2016-09-29 | 2016-12-14 | 宜昌南玻硅材料有限公司 | A kind of detection zone-melted silicon single crystal rod and drawing method thereof |
| WO2017070827A1 (en) * | 2015-10-26 | 2017-05-04 | 北京京运通科技股份有限公司 | Automatic zone melting crystal growth method and system |
| CN108203841A (en) * | 2016-12-20 | 2018-06-26 | 有研半导体材料有限公司 | A kind of method for improving shouldering success rate in zone-melted silicon single crystal growth course |
| CN110318096A (en) * | 2019-06-28 | 2019-10-11 | 北京天能运通晶体技术有限公司 | Zone-melted silicon single crystal ending method and drawing method |
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