CN106222745B - A kind of detection zone-melted silicon single crystal stick and its drawing method - Google Patents
A kind of detection zone-melted silicon single crystal stick and its drawing method Download PDFInfo
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- CN106222745B CN106222745B CN201610863183.9A CN201610863183A CN106222745B CN 106222745 B CN106222745 B CN 106222745B CN 201610863183 A CN201610863183 A CN 201610863183A CN 106222745 B CN106222745 B CN 106222745B
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- single crystal
- silicon single
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- axle speed
- stick
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
Abstract
The invention discloses a kind of detection zone-melted silicon single crystal stick and its drawing method, the crystal orientation of the zone-melted silicon single crystal stick is<111>, and there are three equally distributed crest lines and a crystalline substance bud obviously swelled in outer surface.When drawing, operated under high-purity argon gas atmosphere.Silicon single crystal is set to occur three ribs and a crystalline substance bud obviously swelled during subsequent growth by operation appropriate during seeding, necking down, shouldering.This method can effectively avoid introduced contaminants be introduced into and polysilicon in P elements loss, while the defect concentration of zone-melted silicon single crystal can be greatly reduced, to improve the accuracy of silicon single crystal items detection.Finally improve the accuracy determined polysilicon inherent quality.
Description
Technical field
The invention belongs to polysilicon quality testing field, a kind of detection zone-melted silicon single crystal stick and its drawing are specifically provided
Method.
Background technique
The zone-melted silicon single crystal stick of detection is made according to polycrystalline silicon substrate phosphorus test stone.Generally by drill core or cutting
Cut the polysilicon sample core that is obtained after rounding carry out area's melting and pulling at.In silicon monocrystal growth generally using high-purity argon gas as protection
Polysilicon is drawn into<111>by a series of operation such as preheating thawing, seeding, necking down, shouldering, isodiametric growth, ending by gas
The monocrystalline silicon of crystal orientation.The silicon single crystal bar main part of<111>crystal orientation drawn is cylindrical body, and outer surface is uniformly distributed three ribs
Line.
The intact silicon single crystal of the crest line currently prepared according to polycrystalline silicon substrate phosphorus test stone is lacked there are still more inside it
It falls into.These defects have certain compound action to the minority carrier of silicon crystal, make the apparent minority carrier life time of silicon crystal significantly
It reduces, to influence the accuracy of minority carrier life time measurement；Infrared absorption of the defect more simultaneously to element to be measured in silicon single crystal
The biggish interference of relative line strengths reduces the accuracy of oxygen, carbon, V, III race's detection of content of element.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of detection zone-melted silicon single crystal sticks and its drawing method, can have
Effect avoid introduced contaminants be introduced into and polysilicon in P elements loss, while the defect that zone-melted silicon single crystal can be greatly reduced is close
Degree, to improve the accuracy of silicon single crystal items detection.
In order to solve the above technical problems, the technical scheme adopted by the invention is that: a kind of detection zone-melted silicon single crystal stick,
Crystal orientation is<111>, and there are three equally distributed crest lines and a crystalline substance bud obviously swelled in the outer surface of silicon single crystal bar.
Further, the crystalline substance bud obviously swelled is in the isodiametric growth part of silicon single crystal rod (shouldering is between ending)
The 1-2mm protrusion longitudinally extended.
The invention further relates to draw method of the detection with zone-melted silicon single crystal stick, specific steps are as follows:
1) polycrystalline silicon rod is packed on the sample core fixture in zone melting furnace, seed crystal is fixed in seed holder；
2) it places preheating fork and is passed through argon gas, while preheating to polycrystalline silicon rod after closing fire door vacuumizes；
3) material is carried out after preheating, after polycrystalline silicon rod melting, seed crystal and silicon material are subjected to welding, shaping after welding
And start seeding operation；
4) lower axle decrease speed is set, uniformly increases to 12mm/Min stage by stage from 4mm/Min, meanwhile, it is thick according to seeding
Thin and the position of solid-liquid interface, power per liter to 7.0KV, it is ensured that melting zone is not pulled off or solidifies under current pulling rate, starts thin
Neck growth；
5) should occur three uniform crest lines during seeding, thin neck growth diameter is less than 3mm, length about 30mm30-
35mm, lower axle speed is kept constant in growth course, ensures thin neck according to upper axle speed and power is gently finely tuned the case where material
What is grown is uniform；
6) lower axle speed is reduced simultaneously in two stages to 5mm/Min, axle speed is to 2.5mm/Min in raising；Then will
Power is down to 6.2KV in two stages, starts shouldering；Upper axle speed is reduced after stabilization, observes that the shoulder melting zone that warps is not axis pair
Upper axle speed feed supplement is increased after title；After shouldering is stablized, upper axle speed is recalled into 2.5mm/Min, starts isodiametric growth；
7) behind 12 melting zones of isodiametric growth, start to finish up, when ending reaches desired value to single crystal diameter, by melting zone
It breaks, waits the solidification of tail portion silicon liquid, then power regulation is zeroed, upper and lower axle speed is returned to zero, area is molten to complete, and obtains detection and uses
Zone-melted silicon single crystal stick.
Further, in step 6), in reduction when axle speed, it is reduced to 2.2mm/Min, the degree that shoulder warps is molten
Area bloats 1-2mm to one side, and upper axle speed is increased when feed supplement to 2.8mm/Min.
It is described when being passed through argon gas, it is passed through 99.999% argon gas and guarantees that furnace pressure is being being greater than atmospheric pressure, a flow
18slpm。
Further, the zone melting furnace is the molten inspection furnace in area of model TDL-FZ26A, coil diameter 15mm.
Detection zone-melted silicon single crystal stick provided by the invention, since there are three equally distributed crest lines and one in its outer surface
The crystalline substance bud obviously swelled, the silicon single crystal bar defect concentration of the structure is well below the former columned silicon single crystal of three traditional ribs
Stick.
Drawing method provided by the invention is made during to polycrystalline silicon material seeding, necking down, shouldering by operation appropriate
The defect concentration of silicon single crystal is extremely low, eliminates crystal defect and does to minority carrier life time detection, oxygen, carbon, V, III race's Element detection
It disturbs, improves the accuracy of testing result, so as to improve the accuracy determined polysilicon inherent quality.
Step 4) and 5) seeding, necking down operation in eliminate the dislocation of crystal as far as possible, step 6) passes through shouldering
When conscious operation form brilliant bud and further exclude the defects of crystal to plane of crystal.To reach reduction monocrystalline silicon
The purpose of stick defect concentration.The defect density in silicon single crystal rod can be made to be reduced to 10 at present3-104cm-2, hence it is evident that reduce crystal
Defect is detected to minority carrier life time and the interference of impurity content infrared spectrum analysis.
Detailed description of the invention
Fig. 1 is the cross section of a single crystal figure of the detection zone-melted silicon single crystal stick of comparative example.
Fig. 2 is the cross section of a single crystal figure of detection zone-melted silicon single crystal stick provided by the invention.
Fig. 3 is the isometrical place section preferential etch figure of monocrystalline of the detection zone-melted silicon single crystal stick of comparative example.
Fig. 4 is the isometrical place section preferential etch figure of monocrystalline of detection zone-melted silicon single crystal stick provided by the invention.
Specific embodiment
Below with reference to embodiment, the present invention is furture elucidated.These embodiments be interpreted as being merely to illustrate the present invention and
It is not intended to limit the scope of the invention.After having read the content of the invention recorded, those skilled in the art can be with
The present invention is made various changes or modifications, these equivalence changes and modification equally fall into model defined by claims of the present invention
It encloses.
Embodiment 1:
This method is drawn using molten inspection furnace (coil diameter 15mm) in area of model TDL-FZ26A, including following
Step:
1) polycrystalline silicon rod is packed on the sample core fixture in zone melting furnace, seed crystal is fixed in seed holder；
2) place preheating fork, close after fire door vacuumizes, be passed through 99.999% argon gas and guarantee furnace pressure+
0.01MPa flow is 18slpm.And polysilicon lining bar is heated.
3) material is carried out after preheating, after polycrystalline silicon material melting, seed crystal and silicon material are subjected to welding, shaping after welding
And start seeding operation.
4) lower axle decrease speed is set, uniformly increases to 12mm/Min stage by stage from 4mm/Min.Meanwhile it is thick according to seeding
Thin and the position of solid-liquid interface, power per liter to 7.0KV.Start thin neck growth.
5) should occur three uniform crest lines (3 stains are uniformly distributed at solid liquid interface), thin neck growth during seeding
Diameter should be less than 3mm, length about 30mm.Lower axle speed is kept constant in growth course, on gently finely tuning the case where material
Axle speed and power ensure the uniform of thin neck growth.
6) lower axle speed is reduced simultaneously in two stages to 5mm/Min, axle speed is to 2.5mm/Min in raising；Then will
Power is down to 6.2KV in two stages, starts shouldering.Upper axle speed is slightly reduced after stabilization, is observed after shoulder slowly warps (out
Existing " brilliant bud ") axle speed feed supplement in increasing.After shouldering is stablized, upper axle speed is recalled into 2.5mm/Min, starts isodiametric growth；
7) behind 12 melting zones of isodiametric growth, start to finish up.When ending reaches desired value to single crystal diameter, by melting zone
It breaks.The solidification of tail portion silicon liquid is waited, then power regulation is zeroed, upper and lower axle speed is returned to zero.Qu Rong is completed.
Comparative example: traditional preparation method is not go out brilliant bud during area is molten, and silicon single crystal rod is that three ribs are cylindric.
The cross section of a single crystal figure of the detection that comparative example and embodiment 1 obtain zone-melted silicon single crystal stick is as depicted in figs. 1 and 2,
In, crest line is represented at A, and brilliant bud is represented at B；Seen using the isometrical place section preferential etch photo of the monocrystalline of comparative example and embodiment 1
Fig. 3 and Fig. 4；Caustic solution: to be measured face upward of sample is put into hydrofluoric acid resistant beaker, with the chemical etch polishing liquid of sufficient amount
Submergence is corroded, and so that liquid level is higher by sample about 1cm, etching time 15~20 minutes, is slowly teetertottered.Sample is used after corrosion
Water sufficiently cleans up.
In Fig. 3, visual field: 100 times of amplification factor, area about 1mm2；In figure subtriangular black graphics be crystal orientation <
111 > dislocation；Visual field in Fig. 4: 100 times of amplification factor, area about 1mm2；It can be seen that there is luxuriant monocrystalline ratio close without luxuriant single-crystal fault
Degree substantially reduces.
Claims (4)
1. a kind of detection zone-melted silicon single crystal stick, it is characterised in that: its crystal orientation is<111>, and the outer surface of silicon single crystal bar has three
Equally distributed crest line and a crystalline substance bud obviously swelled；Its defect concentration is 103-104cm-2；The crystalline substance obviously swelled
The 1-2mm protrusion that bud longitudinally extends in the isodiametric growth part of silicon single crystal rod, the isodiametric growth part are shouldering to ending
Between part.
2. drawing the method that zone-melted silicon single crystal stick is used in detection described in claim 1, which is characterized in that specific steps are as follows:
1) polycrystalline silicon rod is packed on the sample core fixture in zone melting furnace, seed crystal is fixed in seed holder；
2) it places preheating fork and is passed through argon gas, while preheating to polycrystalline silicon rod after closing fire door vacuumizes；
3) material is carried out after preheating, after polycrystalline silicon rod melting, seed crystal and silicon material are subjected to welding, shaping and is opened after welding
The operation of beginning seeding；
4) lower axle decrease speed is set, uniformly increases to 12mm/Min stage by stage from 4mm/Min, meanwhile, according to seeding thickness and
The position of solid-liquid interface, power per liter to 7.0KV start thin neck growth；
5) should occur three uniform crest lines during seeding, thin neck growth diameter is less than 3mm, and length 30-35mm was grown
Lower axle speed is kept constant in journey, ensures the uniform of thin neck growth according to upper axle speed and power is gently finely tuned the case where material；
6) lower axle speed is reduced simultaneously in two stages to 5mm/Min, axle speed is to 2.5mm/Min in raising；Then by power
It is down to 6.2KV in two stages, starts shouldering；Upper axle speed is reduced after stabilization, is observed and is increased upper axle speed benefit after shoulder warps
Material；After shouldering is stablized, upper axle speed is recalled into 2.5mm/Min, starts isodiametric growth；In reduction when axle speed, it is reduced to
2.2mm/Min, the degree that shoulder warps are that melting zone to one side bloats 1-2mm, and upper axle speed is increased when feed supplement to 2.8mm/Min；
7) behind 12 melting zones of isodiametric growth, start to finish up, when ending reaches desired value to single crystal diameter, melting zone is drawn
It is disconnected, the solidification of tail portion silicon liquid is waited, then power regulation is zeroed, upper and lower axle speed is returned to zero, area is molten to complete, and obtains detection area
Silicon crystal stick.
3. according to the method described in claim 2, it is characterized by: the area that the zone melting furnace is model TDL-FZ26A is melted
Examine furnace, coil diameter 15mm.
4. according to the method described in claim 2, it is characterized by: being passed through 99.999% when being passed through argon gas in the step 2
Argon gas simultaneously guarantees that furnace pressure is being greater than an atmospheric pressure, flow 18slpm.
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| CN106222745B true CN106222745B (en) | 2019-04-19 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108203841B (en) * | 2016-12-20 | 2020-07-10 | 有研半导体材料有限公司 | Method for improving shouldering success rate in growth process of zone-melting silicon single crystal |
| CN109696345A (en) * | 2019-01-31 | 2019-04-30 | 内蒙古通威高纯晶硅有限公司 | A kind of phosphorus boron sample club head preheating crystal pulling method |
| CN110006841B (en) * | 2019-04-11 | 2022-12-06 | 内蒙古神舟硅业有限责任公司 | Method for detecting O, C, III and V group elements in granular polycrystalline silicon |
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| CN114318498B (en) * | 2021-12-29 | 2022-12-02 | 有研半导体硅材料股份公司 | Shouldering method of zone-melting silicon single crystal |
| CN114540942A (en) * | 2022-03-07 | 2022-05-27 | 陕西有色天宏瑞科硅材料有限责任公司 | Preparation method of zone-melting monocrystalline silicon |
| CN114875495A (en) * | 2022-05-18 | 2022-08-09 | 宁夏中晶半导体材料有限公司 | Method for determining crystal line of 111-crystal-orientation monocrystalline silicon |
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