CN102181919A - Method for controlling resistivity of head of Czochralski silicon - Google Patents
Method for controlling resistivity of head of Czochralski silicon Download PDFInfo
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 114
- 239000010703 silicon Substances 0.000 title claims abstract description 114
- 238000000034 method Methods 0.000 title claims abstract description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 113
- 238000012360 testing method Methods 0.000 claims abstract description 56
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 46
- 239000000956 alloy Substances 0.000 claims abstract description 46
- 239000013078 crystal Substances 0.000 claims description 49
- 238000005259 measurement Methods 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 22
- 239000000523 sample Substances 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 10
- 238000010899 nucleation Methods 0.000 description 19
- 239000002019 doping agent Substances 0.000 description 17
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 16
- 229910052698 phosphorus Inorganic materials 0.000 description 16
- 239000011574 phosphorus Substances 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 16
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 12
- 239000007788 liquid Substances 0.000 description 7
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 241001269238 Data Species 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 230000003698 anagen phase Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- -1 this that is to say Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a method for controlling resistivity of a head of Czochralski silicon. The method mainly comprises the following steps of: 1, preparing a test monocrystal; 2, processing the test monocrystal into a test sample, and testing the resistivity of the test sample; 3, if the resistivity of the test sample does not meet the requirements, working out the mass of doped alloy, and performing secondary doping; and 4, preparing a test monocrystal again, testing the resistivity of the test sample, and if the resistivity of the test sample still does not meet the requirements, performing third or fourth doping until the resistivity meets the requirements. The method has the advantages that: the resistivity of the finished product of monocrystal can be accurately controlled, the deviation between the resistivity of the finished product of silicon monocrystal and the target resistivity is controlled in a range of 1 to 3 ohm.cm, the yield of the finished product of silicon monocrystal is improved by 8 percent, and the cost is lowered by about 20 percent.
Description
Technical field
The present invention relates to the production method of silicon single-crystal, particularly a kind of method of controlling the czochralski silicon monocrystal head resistivity.
Background technology
The traditional method of control single crystal silicon resistivity is that this process of preparation of raw material is controlled, and then according to parameters such as silicon single-crystal target resistivity, single heat charging capacity, polycrystal raw material resistivity, resistance alloys rate, preparation technologies, calculate the proportional quantity (mixing first) of polycrystal raw material and alloy, carrying out raw material shove charge, heat fused, crystal-pulling then, is control method before a kind of typical shove charge.But in silicon single-crystal preparation process subsequently, can't accurately control single crystal silicon resistivity, and influenced by raw material, resistance alloys rate test accuracy and operation deviation etc., often make finished product single crystal silicon resistivity and silicon single-crystal target resistivity serious deviation (8～15 Ω .cm) occur, cause the finished product single crystal silicon resistivity not reach target call, qualification rate is low, cost is high.
Summary of the invention
In order to address the above problem, the resistivity after the shove charge of further accurate control silicon single-crystal, the present invention researches and develops a kind of method of controlling the czochralski silicon monocrystal head resistivity.This method is that resistivity measurement carries out secondary or repeatedly adulterated method per sample in preparation silicon single-crystal sample process.According to having diffusion and solidification theory now as can be known, doping agent is certain rules and is distributed in the whole silicon crystal bar, under the constant situation of preparation technology, dopant distribution can not become yet, and the size of the big or small direct reaction resistivity of concentration of dopant, this that is to say, silicon single-crystal each several part resistivity distribution is corresponding one by one with the distribution of doping agent, also being identical rule distributes, therefore, if the resistivity (head resistivity) of the preliminary growth phase of known silicon single-crystal just can be extrapolated bulk silicon monocrystalline resistivity distribution according to this resistivity, thereby reach the purpose of controlling the silicon single-crystal overall resistivity.
The present invention is according to above-mentioned analytical results, after the silicon raw material melts fully, the specimen that at first prepares minor diameter, short length monocrystalline, and it is carried out resistivity measurement, thereby obtain the head resistivity of silicon single-crystal, calculate the doped alloys quality, carry out secondary subsequently or the operation of repeatedly mixing with this head resistivity, reach the purpose of accurate control silicon single-crystal head resistivity, and then form control fully the silicon single-crystal overall resistivity.
The technical solution used in the present invention is: a kind of method of controlling the czochralski silicon monocrystal head resistivity is characterized in that comprising the steps:
Step 1. raw material carries out the drawing of test silicon monocrystalline after all melting and finishing;
Step 2. after the test silicon crystal-pulling finishes, take out the test silicon monocrystalline, test silicon single-wafer cylinder partial is processed into the plane, obtain specimen;
Step 3. afterwards, the planar section of specimen is carried out resistivity measurement with the four point probe resistivity tester, and record resistivity measurement value;
Step 4. the resistivity measurement value of compare test sample and silicon single-crystal target resistivity value, calculate the resistivity measurement value of specimen and the difference of silicon single-crystal target resistivity, if the resistivity measurement value of specimen is than silicon single-crystal target resistivity value 〉=5 Ω .cm, then carry out the operation of following steps, otherwise the resistivity measurement value of specimen satisfies the requirement of silicon single-crystal target resistivity, directly carries out normal pulling operation;
Step 5. according to the resistivity measurement value of specimen and the difference of silicon single-crystal target resistivity value, calculate required doped alloys quality;
Step 6. the doped alloys that will calculate certain mass mixes in the silicon melt;
Step 7. doped alloys fully melt-blended evenly after, repeat step 1 to step 3, and calculate the resistivity measurement value of specimen and the difference of silicon single-crystal target resistivity value once more;
If step 8. calculate the resistivity measurement value of gained specimen than silicon single-crystal target resistivity value 〉=5 Ω .cm for the second time, then repeat step 5 to step 7, until the resistivity measurement value of specimen than silicon single-crystal target resistivity value＜5 Ω .cm, then stop to mix, the resistivity of specimen satisfies the requirement of silicon single-crystal target resistivity, promptly finishes the control of silicon single-crystal head resistivity.
The invention has the beneficial effects as follows: by implementing this method, can accurately control the finished product single crystal silicon resistivity, make finished product single crystal silicon resistivity and target resistivity deviation control in 1-3 Ω .cm scope, finished silicon monocrystalline qualification rate improves 8%, and cost reduces about 20%.
Description of drawings
Fig. 1 is a test silicon monocrystalline synoptic diagram of the present invention.
Embodiment
Below in conjunction with specific embodiment, further specify the present invention and how to realize.
Embodiment 1: it is Kayex CG6000 vertical pulling stove that silicon single-crystal prepares equipment used, 16 cun thermal fields, 35 kilograms of charging capacitys.Its concrete steps are as follows:
1. preparation of raw material: preparation polycrystalline silicon raw material M
Polycrystalline=35kg, and calculate institute's doped alloys (alloy of doping agent and silicon) mass M according to original resistivity of polycrystalline silicon raw material and prepared silicon single-crystal target resistivity
AlloyPolycrystalline silicon raw material base phosphorus resistivity is ρ among this embodiment
Polycrystalline=1000 Ω .cm, the target resistivity ρ of finished silicon monocrystalline
Target=50 Ω .cm, doping agent alloy (P-Si) electricalresistivity
Alloy=0.04 Ω .cm can calculate phosphorus element content ω in the above-mentioned polycrystalline silicon raw material according to being numbered GB/T 13389-92 " phosphorus single crystal silicon resistivity and concentration of dopant conversion rules are mixed in boron-doping " national standard
Polycrystalline=4.2 * 10
12Atoms/cm
3, target resistivity is phosphorus element content ω in the silicon single-crystal of 50 Ω .cm
Target=8.64 * 10
13Atoms/cm
3, doping agent alloy phosphorus element content ω
Alloy=3.53 * 10
17Atoms/cm
3Therefore, required doping agent alloy mass can be obtained by following formula (1):
(M
Polycrystalline+ M
Alloy) * ω
Target-M
Polycrystalline* ω
Polycrystalline=M
Alloy* ω
Alloy-----------(1)
Because doping agent alloy mass M
AlloyVery little, with respect to the polycrystal raw material mass M
PolycrystallineCan ignore, therefore final gained silicon single-crystal quality can be reduced to polycrystal raw material quality (M
Monocrystalline=M
Polycrystalline+ M
Alloy≈ M
Polycrystalline), with above-mentioned numerical value substitution (1) formula, calculate and should add doping agent alloy mass M in the present embodiment blending process
Alloy=8.17g(i.e. doped alloys quality first).
2. the raw material for preparing is put in the Kayex CG6000 type vertical pulling stove, the heatingization material, after the change material finishes, heating power is adjusted to seeding power (this embodiment seeding power is 55kw), set seeding temperature spot (this embodiment seeding temperature spot is 1450 SP), under this temperature, stable silicon liquation 10 minutes.
3. the drawing of test silicon monocrystalline: seed crystal reduced to silicon liquid level contact, the manual setting pulling rate carries out the seeding operation, for discharging dislocation fully, should make the thin neck length degree of seeding be not less than 1.2 times of test silicon single crystal diameter, the thin neck length degree of seeding is 4cm among this embodiment, and the thin neck diameter of seeding is 3.5mm; Carry out shouldering and the operation of commentaries on classics shoulder after seeding finishes, shouldering speed should be tried one's best slowly, avoids too fast and the generation dislocation, and is also ready for the handled easily of back commentaries on classics shoulder simultaneously; When shoulder diameter acquires a certain degree, to change the shoulder operation in advance, guarantee that the diameter after commentaries on classics is takeed on reaches the requirement of isometrical diameter, isometrical diameter should be controlled between the 2cm-3cm, should be less than 2cm, otherwise because diameter is too little, putting changes shoulder excessive velocities (thermal field decision), causes because of the actually operating difficulty dislocation luxuriant phenomenon of breaking to occur; Isometrical diameter should not surpass 3cm yet simultaneously, otherwise causes the waste in too much raw material and man-hour, finally causes cost to rise.The isometrical diameter of test silicon monocrystalline is 3cm for the 2.8cm(optimum diameter in the present embodiment); Enter isometrical maintenance process after changeing shoulder, electrical path length such as maintenance are answered 〉=4cm, can be processed into specimen smoothly to guarantee the test silicon monocrystalline, and the medium electrical path length of present embodiment is 4.2cm; The operation that finishes up at last, epilog should slowly be carried out, and the control pulling rate makes afterbody become taper, and it is pointed that tail end becomes, and then avoid producing dislocation and cause the failure of test silicon crystal-pulling.
4. the processing of specimen: the test silicon monocrystalline is taken out, after cooling finishes, with oilstone the surface is processed, choose the arc surface (the preferably part between rib and the rib) of test silicon monocrystalline equal-diameter part, it is ground into the plane, the planar size is advisable to be fit to the test of four point probe resistivity tester, be generally 5mm * 5mm size, then with test silicon monocrystalline rotation proper angle, grind next test plane, so grind plane 2-3 of test, so that more number of test points certificate to be provided, grind 3 on plane in the present embodiment altogether, grind and to exert oneself in the planarization process evenly to grind direction and carry out as far as possible, avoid intersecting in opposite directions grinding along a direction, reduce to grind affected layer, to increase the accuracy of resistivity measurement as far as possible.
5. adopt SDY-4 four point probe tester that the specimen of completion of processing is carried out resistivity measurement, the test position is the plane of above-mentioned processing, each plane test three times, get the mean value and the record of three test datas, it is as follows to survey three planar average resistivity data in the present embodiment: 62.1 Ω .cm, 63.6 Ω .cm, 62.7 Ω .cm, get the resistivity value of the mean value 62.8 Ω .cm of above-mentioned three data as specimen again.
6. by above test as can be known, the resistivity value 62.8 Ω .cm of specimen are worth the big 12.8 Ω .cm(differences of 50 Ω .cm than the target resistivity of silicon single-crystal), do not reach the product parameters requirement, need carry out the second time and mix.The content of phosphoric equates with the content of phosphoric in the existing silicon melt in the known prepared specimen, therefore can draw the content of phosphoric in the silicon melt by the resistivity value of specimen, same according to the method in the preparation raw material step, according to being numbered the content ω that GB/T 13389-92 " phosphorus single crystal silicon resistivity and concentration of dopant conversion rules are mixed in boron-doping " national standard can calculate phosphoric in silicon melt this moment
Melt=6.83 * 10
13Atoms/cm
3, phosphorus element content ω in institute's doped alloys as can be known secondly
Alloy=3.53 * 10
17Atoms/cm
3, phosphorus element content ω in the target melt
Target=8.64 * 10
13Atoms/cm
3, melt quality can approximate batching quality, i.e. M
Melt≈ M
Polycrystalline+ M
AlloySo=35kg is by following formula: (M
Polycrystalline+ M
Alloy) * ω
Target– M
Melt* ω
Melt=M
Secondary alloy* ω
AlloyCalculating can obtain: M
Secondary alloy=1.79g.
7. adjust the silicon liquid temp, carrying out the silicon bowl draws, after the preparation of silicon bowl finishes, close plate valve in the stove, to last furnace chamber inflation, open fire door, load weighted doped alloys 1.79g is put in the silicon bowl, closes fire door and carry out replacement operator, after displacement finishes, the silicon bowl that carries doped alloys is immersed in the silicon liquid, finish for the second time and mix.
8. after secondary doping finishes, carry out steady temperature operation once more, set seeding temperature spot (this embodiment seeding temperature spot is 1450 SP), under this temperature, stable silicon liquid temp 10 minutes.
9. afterwards, carry out the drawing of test silicon monocrystalline once more according to above-mentioned the 1st～5 step, the processing of specimen, the resistivity measurement of specimen, the resistivity value that finally obtains the specimen behind the secondary doping is 51.8 Ω .cm, be worth the big 1.8 Ω .cm(differences of 50 Ω .cm than silicon single-crystal target resistivity), phase difference＜5 Ω .cm satisfies the requirement of silicon single-crystal target resistivity.
10. according to the 51.8 Ω .cm of the specimen resistivity value behind the above secondary doping, the P constituent content is 8.3 * 10 in melt this moment as can be known
13Atoms/cm
3, and can judge that thus the melt after the doping satisfies the requirement that draws the finished product single crystal silicon resistivity, so operation afterwards can be prepared the finished silicon monocrystalline that resistivity meets the demands according to the czochralski silicon monocrystal preparation technology of routine.
Embodiment 2: it is Kayex CG6000 vertical pulling stove that silicon single-crystal prepares equipment used, 18 cun thermal fields, 55 kilograms of charging capacitys.Its concrete steps are as follows:
1. preparation of raw material: preparation polycrystalline silicon raw material M
Polycrystalline=55kg, its basic phosphorus resistivity is ρ
Polycrystalline=1200 Ω .cm, the target resistivity ρ of expection finished silicon monocrystalline
Target=28 Ω .cm, doping agent alloy (P-Si) electricalresistivity
Alloy=0.04 Ω .cm can calculate phosphorus element content ω in the above-mentioned polysilicon according to being numbered GB/T 13389-92 " phosphorus single crystal silicon resistivity and concentration of dopant conversion rules are mixed in boron-doping " national standard
Polycrystalline=3.5 * 10
12Atoms/cm
3, target resistivity is phosphorus element content ω in the silicon single-crystal of 28 Ω .cm
Target=1.56 * 10
14Atoms/cm
3, doping agent alloy phosphorus element content ω
Alloy=3.53 * 10
17Atoms/cm
3Therefore, required doping agent alloy mass can obtain M by following formula (1)
Alloy=23.8g(i.e. doped alloys quality first).
2. the raw material for preparing is put in the Kayex CG6000 type vertical pulling stove, the heatingization material, after the change material finishes, heating power is adjusted to seeding power (this embodiment seeding power is 55kw), set seeding temperature spot (this embodiment seeding temperature spot is 1450 SP), under this temperature, stable silicon liquation 10 minutes.
3. the drawing of test monocrystalline: test the drawing of monocrystalline according to the method among the embodiment 1, the thin neck length degree of seeding is 3.8cm among this embodiment, the thin neck diameter of seeding is 3.3mm, the isometrical diameter of test silicon monocrystalline is 3cm for the 3cm(optimum diameter), etc. electrical path length is 4.5cm, the operation that finishes up at last, and epilog should slowly be carried out, make afterbody become taper, it is pointed that tail end becomes.
4. the processing of specimen: the test silicon monocrystalline is taken out, after cooling finishes, with oilstone the surface is processed, the arc surface of choosing test monocrystalline equal-diameter part grinds into the plane with it, and the planar size is advisable to be fit to the test of four point probe resistivity tester, is generally 5mm * 5mm size, to test monocrystalline rotation proper angle then, grind next test plane, so grind plane 2-3 of test, grind 3 on plane in the present embodiment altogether.
5. the specimen of completion of processing is carried out resistivity measurement, the test position is the plane of above-mentioned processing, each plane test three times, get the mean value and the record of three secondary flat test datas, it is as follows to survey three planar average resistivity data in the present embodiment: 44 Ω .cm, 43.8 Ω .cm, 43.8 Ω .cm, get the resistivity value of the mean value 43.9 Ω .cm of above-mentioned three data as this specimen again.
6. by above test as can be known, specimen resistivity value 43.9 Ω .cm and target resistivity are worth 28 Ω .cm and differ 15.9 Ω .cm, and phase difference＞5 Ω .cm does not reach the product parameters requirement, need carry out the second time and mix.The content of phosphoric equates with the content of phosphoric in the existing silicon melt in the known prepared specimen, therefore can draw the content of phosphoric in the silicon melt by the resistivity value of specimen, same according to the method in the preparation raw material step, according to being numbered the content ω that GB/T 13389-92 " phosphorus single crystal silicon resistivity and concentration of dopant conversion rules are mixed in boron-doping " national standard can calculate phosphoric in silicon melt this moment
Melt=9.83 * 10
13Atoms/cm
3, phosphorus element content ω in institute's doped alloys as can be known secondly
Alloy=3.53 * 10
17Atoms/cm
3, phosphorus element content ω in the target melt
Target=1.56 * 10
14Atoms/cm
3, melt quality can approximate batching quality, i.e. M
Melt≈ M
Polycrystalline+ M
AlloySo=55kg is by following formula (M
Polycrystalline+ M
Alloy) * ω
Target– M
Melt* ω
Melt=M
Secondary alloy* ω
AlloyCalculating can obtain: M
Secondary alloy=8.99g.
7. adjust the silicon liquid temp, carrying out the silicon bowl draws, after the preparation of silicon bowl finishes, close plate valve in the stove, to last furnace chamber inflation, open fire door, load weighted doped alloys 8.99g is put in the silicon bowl, closes fire door and carry out replacement operator, after displacement finishes, the silicon bowl that carries doped alloys is immersed in the silicon liquid, finish for the second time and mix.
8. after secondary doping finishes, carry out steady temperature operation once more, set seeding temperature spot (this embodiment seeding temperature spot is 1450 SP), under this temperature, stable silicon liquid temp 10 minutes.
9. afterwards, carry out the drawing of test silicon monocrystalline once more according to above-mentioned the 1st～5 step, the processing of specimen, the resistivity measurement of specimen, the resistivity value that finally obtains the specimen behind the secondary doping is 33.2 Ω .cm, be worth 28 Ω .cm with the silicon single-crystal target resistivity and differ 5.2 Ω .cm, phase difference＞5 Ω .cm does not satisfy the requirement of silicon single-crystal target resistivity.
10. because the discontented sufficient requirement of above-mentioned resistivity difference, thus to mix for the third time, same according to above-mentioned method of calculation, doped alloys quality is for the third time calculated: M
Three alloys=3.74g.
After 11. doping finishes for the third time, according to above-mentioned the 1st～5 step, carry out operations such as steady temperature, test single crystal preparation, specimen processing once more, finally obtaining this specimen resistivity is 28.8 Ω .cm, be worth 28 Ω .cm with the silicon single-crystal target resistivity and differ 0.8 Ω .cm, phase difference＜5 Ω .cm satisfies the requirement of silicon single-crystal target resistivity.
12. according to the 28.8 Ω .cm of the specimen resistivity value behind the above secondary doping, the P constituent content is 1.5 * 10 in melt this moment as can be known
14Atoms/cm
3, and can judge that thus the melt after the doping satisfies the requirement that draws the finished product single crystal silicon resistivity, so operation afterwards can be prepared the finished silicon monocrystalline that resistivity meets the demands according to the czochralski silicon monocrystal preparation technology of routine.
Claims (2)
1. a method of controlling the czochralski silicon monocrystal head resistivity is characterized in that comprising the steps:
Step 1. raw material carries out the drawing of test silicon monocrystalline after all melting and finishing;
Step 2. after the test silicon crystal-pulling finishes, take out the test silicon monocrystalline, test silicon single-wafer cylinder partial is processed into the plane, obtain specimen;
Step 3. afterwards, the planar section of specimen is carried out resistivity measurement with the four point probe resistivity tester, and record resistivity measurement value;
Step 4. the resistivity measurement value of compare test sample and silicon single-crystal target resistivity value, calculate the resistivity measurement value of specimen and the difference of silicon single-crystal target resistivity, if the resistivity measurement value of specimen is than silicon single-crystal target resistivity value 〉=5 Ω .cm, then carry out the operation of following steps, otherwise the resistivity measurement value of specimen satisfies the requirement of silicon single-crystal target resistivity, directly carries out normal pulling operation;
Step 5. according to the resistivity measurement value of specimen and the difference of silicon single-crystal target resistivity value, calculate required doped alloys quality;
Step 6. the doped alloys that will calculate certain mass mixes in the silicon melt;
Step 7. doped alloys fully melt-blended evenly after, repeat step 1 to step 3, and calculate the resistivity measurement value of specimen and the difference of silicon single-crystal target resistivity value once more;
If step 8. calculate the resistivity measurement value of gained specimen than silicon single-crystal target resistivity value 〉=5 Ω .cm for the second time, then repeat step 5 to step 7, until the resistivity measurement value of specimen than silicon single-crystal target resistivity value＜5 Ω .cm, then stop to mix, the resistivity of specimen satisfies the requirement of silicon single-crystal target resistivity, promptly finishes the control of silicon single-crystal head resistivity.
2. a kind of method of controlling the czochralski silicon monocrystal head resistivity according to claim 1, it is characterized in that: the length of described test silicon crystal-pulling is answered 〉=6cm, the length of test silicon crystal-pulling comprises shouldering part, equal-diameter part and ending part, wherein the equal-diameter part diameter is 2cm～3cm, equal-diameter part length 〉=4cm.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654804A (en) * | 2009-09-24 | 2010-02-24 | 浙江大学 | Method for controlling specific resistance of gallium-doped Czochralski silicon in crystal growth process |
| CN101906659A (en) * | 2010-08-18 | 2010-12-08 | 高佳太阳能股份有限公司 | Doping method of monocrystalline silicon for photovoltaics |
-
2011
- 2011-04-13 CN CN 201110092541 patent/CN102181919B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654804A (en) * | 2009-09-24 | 2010-02-24 | 浙江大学 | Method for controlling specific resistance of gallium-doped Czochralski silicon in crystal growth process |
| CN101906659A (en) * | 2010-08-18 | 2010-12-08 | 高佳太阳能股份有限公司 | Doping method of monocrystalline silicon for photovoltaics |
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