CN104911694A - Doping process for production of silicon single crystal rods - Google Patents
Doping process for production of silicon single crystal rods Download PDFInfo
- Publication number
- CN104911694A CN104911694A CN201510291711.3A CN201510291711A CN104911694A CN 104911694 A CN104911694 A CN 104911694A CN 201510291711 A CN201510291711 A CN 201510291711A CN 104911694 A CN104911694 A CN 104911694A
- Authority
- CN
- China
- Prior art keywords
- raw material
- single crystal
- group element
- boron group
- casing drum
- 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
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a doping process for the production of silicon single crystal rods, which comprises the operation steps of raw material preparation, feeding for the first time, feeding for the second time, heating and melting, and the like. By changing the doping method and doping time of a boron group element alloy, the distance between the head part and tail part of a silicon single crystal rod is controlled and shortened, the balance internal of the electrical resistivity of the silicon single crystal rod is reduced, the length of the high-quality section of the silicon single crystal rod is increased, and the yield of the silicon single crystal rod is improved.
Description
Technical field
The present invention relates to a kind of silicon single crystal rod production technique, especially a kind of doping process adopting pulling of crystals manufacturing process produce single crystal silicon rod.
Background technology
Current silicon single-crystal adopts pulling of crystals manufacturing process and CZ method to produce usually, the specific embodiment that CZ method is produced comprises charging and melt, welding, thin neck, shouldering, turn take on, isodiametric growth and ending several stage.Charging and melt stage are the first stages of CZ method, and the operation of this one-phase is often related to the success or failure of process of growth, directly affects the production of monocrystalline.
CZ method is in charging and melt stage, and usually will add the impurity element of some amount, this step is called doping.In CZ method technique, the resistivity of silicon single crystal is the important factor determining monocrystalline quality, and silicon single crystal resistivity is adjusted by admixture boron group element, and boron group element addition content too much can cause the resistivity of silicon single crystal on the low side; Boron group element addition content is crossed and is easily caused the resistivity of silicon single crystal higher at least.Even if boron group element addition content is suitable, because doping efficiency is very low, only have a little boron group element can enter in silicon crystal, most boron group element is suspended state in melt silicon, and current boron group element adding technology is mainly added in the bottom of quartz crucible at when filling with substance whole boron group element alloy, this just causes boron group element in melt silicon, spread inequality, the head and tail portion resistivity difference of producing the silicon single crystal rod obtained is larger, usually because boron group element is deposited on bottom, the resistivity head height afterbody of silicon single crystal rod is low.Simultaneously comparatively large between differential resistivity frontal region, cause silicon single crystal rod ratio within the scope of optimal resistivity few.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of doping process produced for silicon single crystal rod, prevents boron group element to be deposited on the bottom of melt silicon, reduces resistivity difference, improves the seed output and quality of silicon single crystal rod.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
For the doping process that silicon single crystal rod is produced, comprise the following steps:
A, preparation raw material: take total raw material and boron group element alloy, total raw material comprises crystal tankage and polycrystal, wherein crystal tankage: the weight ratio of polycrystal is 2:3-1:1, total raw material is divided into two parts, wherein first part of raw material is whole crystal tankage and the polycrystal of 50-60%, and second part of raw material is the polycrystal of remaining 40-50%;
B, first fuel loading: all loaded in quartz crucible by first part of raw material, put into the main furnace chamber of single crystal growing furnace afterwards, close main furnace chamber by quartz crucible;
C, second time charging: second part of raw material is added in casing drum, time between 3/2 to four/3rds of loading second part of raw material weight, boron group element alloy is slowly added in casing drum, after afterwards remaining second part of raw material all being loaded casing drum, casing drum is lifted the concubine to single crystal growing furnace;
D, heat fused: single crystal growing furnace closes stove and finds time, heat temperature raising is started when vacuum tightness in single crystal growing furnace reaches after below 10Pa, after part raw material of first in quartz crucible is all melted into melt silicon, casing drum is moved to above melt silicone liquid level, part raw material of second in casing drum and boron group element alloy are all added in quartz crucible;
E, after the total raw material in quartz crucible and boron group element alloy have all melted, adjustment Heating temperature is to temperature of craning one, and crucible rotary speed, to required crucible position of craning one, is improved in adjustment crucible position, takes out casing drum and also installs seed crystal, carries out follow-up crystal pulling and produces.
The further improvement of the above-mentioned doping process for silicon single crystal rod production is: in described steps A, the diameter of the polycrystal of second part of raw material is 5-25mm.
The above-mentioned further improvement of doping process of producing for silicon single crystal rod is: in described step C, keep when adding boron group element alloy boron group element alloy not with casing drum sidewall contact.
The beneficial effect adopting technique scheme to produce is:
The present invention is by changing adulteration method and the admixture time of boron group element alloy, boron group element alloy is added in melt silicon, alloy is prevented constantly to precipitate at the bottom of crucible in single crystal growth process, the gap controlling and shorten between silicon single crystal rod head and afterbody, the difference reducing silicon single crystal rod resistivity is interval, add the length of silicon single crystal rod high-quality section, improve the output of silicon single crystal rod.
The present invention is simple to operate, decreases the addition content of boron group element alloy, thus decreases the introducing of Crystal impurity, improves the cleanliness factor of raw material, improves output and yield rate.
Note when adding second part of boron group element alloy boron group element alloy can not with the sidewall contact of casing drum, avoid boron group element alloy in subsequent heat process to stick on casing drum barrel due to high temperature melting, cannot add to smoothly in melt silicon.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
For the doping process that silicon single crystal rod is produced, comprise the following steps:
A, preparation raw material: resistivity as requested carries out total raw material proportioning, total raw material comprises crystal tankage and polycrystal, wherein, crystal tankage: the weight ratio of polycrystal carries out proportioning according to the ratio of 2:3-1:1, calculate the boron group element alloy amount needing to add according to the universal calculation equation of alloy requirement, calculation formula is:
Boron group element alloy amount=[target resistivity corresponding atom number * total raw material weight/segregation coefficient-(the corresponding atom number of crystal tankage weight * crystal offal resistivity)]/alloy concentrations;
The corresponding atom number of target resistivity in formula and segregation coefficient are constant.
Take total raw material and the boron group element alloy needing to use as requested, total raw material is divided into first part of raw material and second part of raw material, wherein first part of raw material is whole crystal tankage and the polycrystal of 50-60%, second part of raw material is the polycrystal of remaining 40-50%, wherein the diameter of the polycrystal of second part of raw material is 5-25mm, facilitates melting.
B, first fuel loading: first part of raw material is by volume divided into dead small, middle block of material and bulk material in size Distribution Area, the dead small that one deck volume that tiles bottom quartz crucible is relatively little, dead small is placed the relatively large bulk material of volume and middle block of material, bulk material in quartz crucible install to account for quartz crucible volume 2/1 to three/2nds between time, pour dead small into, dead small is utilized to be filled up in the gap between bulk material, so conveniently hold more raw material, continue after the gap is filled in quartz crucible, drop into remaining first part of raw material.
First part of raw material all loads after in quartz crucible, quartz crucible is put into the main furnace chamber of single crystal growing furnace, closes main furnace chamber;
C, second time charging: first the casing drum of quartzy material is cleaned out, afterwards second part of raw material is added in casing drum;
C1, add boron group element alloy: be housed to second part of raw material weight 3/2 to four/3rds between time, boron group element alloy is slowly added in casing drum, note when adding boron group element alloy boron group element alloy can not with the sidewall contact of casing drum, avoid sticking on casing drum barrel after the fusing of boron group element alloy high-temp in subsequent heat process, cannot add in melt silicon.After boron group element has added, continue to load remaining second part of raw material toward casing drum.
After having feeded, casing drum is lifted into the concubine of single crystal growing furnace.
D, heat fused: single crystal growing furnace closes stove and finds time, detect the vacuum tightness in single crystal growing furnace.After the vacuum tightness in single crystal growing furnace reaches below 10Pa, start heat temperature raising.After part raw material of first in quartz crucible is all melted into melt silicon, casing drum is moved to the ullage of melt silicon, part raw material of second in casing drum and boron group element alloy are all added in quartz crucible, continue heat fused.
E, after the total raw material in quartz crucible and boron group element alloy have all melted, adjustment Heating temperature is to temperature of craning one, and crucible rotary speed, to required crucible position of craning one, is improved in adjustment crucible position, takes out casing drum and also installs seed crystal, carries out follow-up crystal pulling and produces.
After using doping process of the present invention to carry out silicon single crystal rod production, reduce boron group element alloy dosage about 12%, reduce production cost.Reduce between the resistivity zone at the silicon single crystal rod two ends that production obtains, the resistivity value of bonding crystalline silicon rod is in optimum range, improves product quality.
Claims (3)
1., for the doping process that silicon single crystal rod is produced, it is characterized in that comprising the following steps:
A, preparation raw material: take total raw material and boron group element alloy, total raw material comprises crystal tankage and polycrystal, wherein crystal tankage: the weight ratio of polycrystal is 2:3-1:1, total raw material is divided into two parts, wherein first part of raw material is whole crystal tankage and the polycrystal of 50-60%, and second part of raw material is the polycrystal of remaining 40-50%;
B, first fuel loading: all loaded in quartz crucible by first part of raw material, put into the main furnace chamber of single crystal growing furnace afterwards, close main furnace chamber by quartz crucible;
C, second time charging: second part of raw material is added in casing drum, time between 3/2 to four/3rds of loading second part of raw material weight, boron group element alloy is slowly added in casing drum, after afterwards remaining second part of raw material all being loaded casing drum, casing drum is lifted the concubine to single crystal growing furnace;
D, heat fused: single crystal growing furnace closes stove and finds time, heat temperature raising is started when vacuum tightness in single crystal growing furnace reaches after below 10Pa, after part raw material of first in quartz crucible is all melted into melt silicon, casing drum is moved to above melt silicone liquid level, part raw material of second in casing drum and boron group element alloy are all added in quartz crucible;
E, after the total raw material in quartz crucible and boron group element alloy have all melted, adjustment Heating temperature is to temperature of craning one, and crucible rotary speed, to required crucible position of craning one, is improved in adjustment crucible position, takes out casing drum and also installs seed crystal, carries out follow-up crystal pulling and produces.
2. the doping process produced for silicon single crystal rod according to claim 1, it is characterized in that: in described steps A, the diameter of the polycrystal of second part of raw material is 5-25mm.
3. the doping process produced for silicon single crystal rod according to claim 1, is characterized in that: in described step C, keep when adding boron group element alloy boron group element alloy not with casing drum sidewall contact.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510291711.3A CN104911694A (en) | 2015-06-01 | 2015-06-01 | Doping process for production of silicon single crystal rods |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510291711.3A CN104911694A (en) | 2015-06-01 | 2015-06-01 | Doping process for production of silicon single crystal rods |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104911694A true CN104911694A (en) | 2015-09-16 |
Family
ID=54081120
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510291711.3A Pending CN104911694A (en) | 2015-06-01 | 2015-06-01 | Doping process for production of silicon single crystal rods |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104911694A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105200513A (en) * | 2015-10-19 | 2015-12-30 | 天津市环欧半导体材料技术有限公司 | Novel Czochralski silicon single crystal doping method with resistivity control function |
| CN105755533A (en) * | 2016-05-20 | 2016-07-13 | 麦斯克电子材料有限公司 | Method for preparing high-resistance silicon single crystal by Czochralski method |
| CN106012010A (en) * | 2016-08-15 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Method and apparatus for secondary addition of doping agent |
| CN106757313A (en) * | 2016-12-29 | 2017-05-31 | 上海合晶硅材料有限公司 | It is overweight to mix arsenic crystal bar drawing method |
| CN107460538A (en) * | 2017-07-19 | 2017-12-12 | 内蒙古中环光伏材料有限公司 | It is a kind of to improve the method for throwing monocrystalline silicon crystal forming rate again and the material block for launching barium carbonate |
| CN112760704A (en) * | 2020-12-28 | 2021-05-07 | 晶澳太阳能有限公司 | Boron-gallium co-doped single crystal preparation equipment and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005007941A1 (en) * | 2003-07-18 | 2005-01-27 | Jianzhong Yuan | An apparatus and method for recharge raw material |
| JP2010013314A (en) * | 2008-07-03 | 2010-01-21 | Sumco Corp | Method and apparatus for growing silicon single crystal |
| CN102094236A (en) * | 2010-12-22 | 2011-06-15 | 任丙彦 | Czochralski method for growing long-lifetime P-type boron-doped silicon single crystal |
| CN102296352A (en) * | 2011-08-16 | 2011-12-28 | 北京京运通科技股份有限公司 | Ingot casting method for single polysilicon of 800kg |
| CN102345157A (en) * | 2011-10-09 | 2012-02-08 | 内蒙古中环光伏材料有限公司 | Continuous re-feeding production method of solar-grade Czochralski silicon |
| CN102758253A (en) * | 2012-06-20 | 2012-10-31 | 合肥景坤新能源有限公司 | Czochralski polycrystalline silicon or monocrystal silicon preparation technology |
| CN103074681A (en) * | 2013-02-17 | 2013-05-01 | 英利集团有限公司 | Secondary feeding method |
-
2015
- 2015-06-01 CN CN201510291711.3A patent/CN104911694A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005007941A1 (en) * | 2003-07-18 | 2005-01-27 | Jianzhong Yuan | An apparatus and method for recharge raw material |
| JP2010013314A (en) * | 2008-07-03 | 2010-01-21 | Sumco Corp | Method and apparatus for growing silicon single crystal |
| CN102094236A (en) * | 2010-12-22 | 2011-06-15 | 任丙彦 | Czochralski method for growing long-lifetime P-type boron-doped silicon single crystal |
| CN102296352A (en) * | 2011-08-16 | 2011-12-28 | 北京京运通科技股份有限公司 | Ingot casting method for single polysilicon of 800kg |
| CN102345157A (en) * | 2011-10-09 | 2012-02-08 | 内蒙古中环光伏材料有限公司 | Continuous re-feeding production method of solar-grade Czochralski silicon |
| CN102758253A (en) * | 2012-06-20 | 2012-10-31 | 合肥景坤新能源有限公司 | Czochralski polycrystalline silicon or monocrystal silicon preparation technology |
| CN103074681A (en) * | 2013-02-17 | 2013-05-01 | 英利集团有限公司 | Secondary feeding method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105200513A (en) * | 2015-10-19 | 2015-12-30 | 天津市环欧半导体材料技术有限公司 | Novel Czochralski silicon single crystal doping method with resistivity control function |
| CN105755533A (en) * | 2016-05-20 | 2016-07-13 | 麦斯克电子材料有限公司 | Method for preparing high-resistance silicon single crystal by Czochralski method |
| CN106012010A (en) * | 2016-08-15 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Method and apparatus for secondary addition of doping agent |
| CN106757313A (en) * | 2016-12-29 | 2017-05-31 | 上海合晶硅材料有限公司 | It is overweight to mix arsenic crystal bar drawing method |
| CN107460538A (en) * | 2017-07-19 | 2017-12-12 | 内蒙古中环光伏材料有限公司 | It is a kind of to improve the method for throwing monocrystalline silicon crystal forming rate again and the material block for launching barium carbonate |
| CN112760704A (en) * | 2020-12-28 | 2021-05-07 | 晶澳太阳能有限公司 | Boron-gallium co-doped single crystal preparation equipment and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104911694A (en) | Doping process for production of silicon single crystal rods | |
| KR101939594B1 (en) | Growth of a uniformly doped silicon ingot by doping only the initial charge | |
| TWI745520B (en) | Methods for forming single crystal silicon ingots with improved resistivity control | |
| CN105755532A (en) | Crystalline silicon preparation method and crystalline silicon | |
| US9885122B2 (en) | Method of manufacturing silicon single crystal | |
| CN106795647A (en) | Resistivity control method and N-shaped monocrystalline silicon | |
| CN101724891B (en) | Automatic compensation method for diameter of czochralski silicon monocrystalline | |
| JP6299543B2 (en) | Resistivity control method and additional dopant injection device | |
| CN105887193A (en) | Silicone single crystal growth technique with uniform axial electrical resistivity | |
| CN102995108A (en) | Continuous charging silicon single crystal furnace | |
| CN103215633A (en) | Method for casting ingots by polycrystalline silicon | |
| KR102054383B1 (en) | Method for producing silicon single crystal | |
| CN110983427A (en) | Repeated segment taking and re-casting process for large-diameter single crystal silicon rod | |
| CN104846437B (en) | What resistivity was evenly distributed mixes gallium crystalline silicon and preparation method thereof | |
| JP4830312B2 (en) | Compound semiconductor single crystal and manufacturing method thereof | |
| CN104451872A (en) | Production method of solar-grade czochralski silicon | |
| JP5170061B2 (en) | Resistivity calculation program and single crystal manufacturing method | |
| CN104746134B (en) | Using the n-type pulling single crystal silicon method of compensation silicon material | |
| CN202099408U (en) | Biquartz crucible device used for producing czochralski silicon single crystal | |
| CN101812726A (en) | Method for preparing gallium-doped p-type crystalline silicon | |
| JP5370394B2 (en) | Compound semiconductor single crystal substrate | |
| CN103397378A (en) | Preparation method of polycrystalline silicon ingot | |
| CN104313681A (en) | Device for growth of multinary compound crystals and application thereof | |
| CN102168302B (en) | Double-quartz-crucible device and method for producing czochralski silicon single crystal | |
| CN201545932U (en) | Silica crucible dedicated for preparation of mercury indium telluride (MIT) single crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150916 |
|
| RJ01 | Rejection of invention patent application after publication |