CN102912424B - Method for improving uniformity of axial resistivity of czochralski silicon and obtained monocrystalline silicon - Google Patents
Method for improving uniformity of axial resistivity of czochralski silicon and obtained monocrystalline silicon Download PDFInfo
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 60
- 239000010703 silicon Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title description 26
- 239000007789 gas Substances 0.000 claims abstract description 61
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000013078 crystal Substances 0.000 claims abstract description 49
- 239000002019 doping agent Substances 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 18
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 3
- 238000002844 melting Methods 0.000 claims abstract description 3
- 230000008018 melting Effects 0.000 claims abstract description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical group [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 14
- 229910052733 gallium Inorganic materials 0.000 claims description 14
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 10
- 229910052787 antimony Inorganic materials 0.000 claims description 9
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical group [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 9
- 239000005922 Phosphane Substances 0.000 claims description 2
- 229910000064 phosphane Inorganic materials 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 20
- 229910052786 argon Inorganic materials 0.000 description 10
- 238000005204 segregation Methods 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 5
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 4
- 229920005591 polysilicon Polymers 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004377 microelectronic Methods 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- XGCTUKUCGUNZDN-UHFFFAOYSA-N [B].O=O Chemical compound [B].O=O XGCTUKUCGUNZDN-UHFFFAOYSA-N 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for improving the uniformity of axial resistivity of czochralski silicon. The method comprises the steps as follows: (1) melting a polycrystalline silicon raw material and a solid doping agent in an argon atmosphere to obtain stable molten silicon; (2) introducing seed crystals into the stable molten silicon, and conducting constant diameter growth on the crystals after necking and shouldering processes; and (3) during the constant diameter growth period, adding dopant gas with the conductive type opposite to that of the solid doping agent until the growth of the czochralski silicon is fulfilled. According to the method, the type and the usage amount of the dopant gas are convenient to control, various required impurity concentration distributions can be obtained, the utilization rate of the czochralski silicon is increased, and the uniformity of the resistivity of the czochralski silicon is remarkably improved.
Description
Technical Field
The invention relates to the field of semiconductor materials, in particular to a method for improving the uniformity of the axial resistivity of czochralski monocrystalline silicon by a gas-phase doping method and the monocrystalline silicon obtained by the method.
Background
Photovoltaic power generation is the most important renewable energy technology in the foreseeable future. Photovoltaic power generation in 2030 will meet nearly 10% of the global power demand as predicted by the European Photovoltaic Industry Association (EPIA).
The current solar cell is mainly manufactured based on a boron-doped monocrystalline silicon material, but because the monocrystalline silicon contains boron and oxygen at the same time, a boron-oxygen complex is formed in the use process of the solar cell, so that the photoelectric conversion efficiency of the solar cell is reduced by more than 10%, and the performance of the solar cell is remarkably reduced. To solve this problem, researchers have invented gallium-doped monocrystalline silicon solar cells.
Although the gallium-doped monocrystalline silicon solar cell has no light attenuation phenomenon, the gallium-doped monocrystalline silicon solar cell has great defects, because the segregation coefficient of gallium in silicon is extremely low (about 0.008), the axial resistivity difference is great in the growth process of the gallium-doped monocrystalline silicon, the resistivity of the finally grown monocrystalline silicon in the monocrystalline silicon cannot meet the requirement, and the actual utilization rate of the gallium-doped monocrystalline silicon is only about 80%.
In addition, the resistivity distribution of the gallium-doped czochralski silicon is wide, so that the efficiency distribution of the solar cell is also wide, and the consistency of the power output of the solar cell module is seriously influenced.
These drawbacks result in gallium-doped solar cells that are expensive and difficult to implement on a large scale in the industry. So far, no effective means is published at home and abroad to obtain the gallium-doped Czochralski silicon with uniformly distributed axial resistivity.
In the field of microelectronics, the heavily antimony-doped Czochralski monocrystalline silicon is also an important material, and an n/n + epitaxial wafer prepared from the heavily antimony-doped Czochralski monocrystalline silicon has the advantages of narrow transition region, steep junction gradient, small diffusion coefficient of antimony at high temperature and the like, so that the antimony-doped monocrystalline silicon becomes an important substrate.
However, like gallium-doped single crystal silicon, the equilibrium segregation coefficient of antimony in silicon is also very small (about 0.023), again resulting in poor uniformity of the axial resistivity of antimony-doped czochralski silicon.
Disclosure of Invention
The invention provides a method for improving the uniformity of the axial resistivity of czochralski silicon, which greatly improves the uniformity of the axial resistivity of the czochralski silicon by a gas-phase doping method, is simple and practical and has good industrial application prospect.
A method for improving the uniformity of the axial resistivity of czochralski silicon comprises the following steps:
(1) melting a polycrystalline silicon raw material and a solid dopant in an argon atmosphere to obtain stable molten silicon;
(2) introducing seed crystals into the stable molten silicon, and leading the crystal growth to enter an isodiametric growth stage through necking and shouldering processes;
(3) and in the isometric growth stage, introducing doping gas with the conductivity type opposite to that of the solid dopant until the growth of the Czochralski silicon is finished.
In the normal equal-diameter growth process of the czochralski silicon single crystal, doping gas is continuously and uniformly introduced to realize gas-phase doping, and the distribution of gas-phase impurities introduced by the doping gas in the silicon single crystal obeys the following equation:
wherein,
Csis the doping concentration of impurities in the silicon single crystal;
a is the doping rate of the doping gas;
v is the growth rate of the czochralski silicon;
k is the segregation coefficient of impurities introduced by the doping gas;
g is the coagulation fraction.
If p-type and n-type impurities are co-doped, the distribution of carriers in the silicon crystal obeys the following equation (taking p-type gallium and n-type phosphorus as an example):
wherein,
p is the concentration of carriers in the silicon crystal;
C0is the initial melt concentration of gallium;
k1is the segregation coefficient of gallium;
g is the coagulation fraction;
a is a doping rate of the doping gas (amount of impurities introduced per unit time, flow rate by the doping gas);
v is the growth rate of the czochralski silicon;
k2is the segregation coefficient of phosphorus;
represents the impurity concentration introduced by the solid dopant;
indicating the concentration of the dopant gas introduced impurity.
By adjusting the concentration and the flow of the doping gas, the optimal gas phase doping amount can be obtained, and the axial resistivity of the czochralski silicon single crystal is kept uniformly distributed.
The optimal gas doping amount is as follows:
wherein,
C0is the initial melt concentration of the solid dopant;
k1is the segregation coefficient of the solid dopant;
a is the doping rate of the doping gas;
v is the growth rate of the czochralski silicon;
k2is the segregation coefficient of impurities in the doping gas.
According to this formula, a suitable amount of phosphane to be doped in compensated crystals of gallium and phosphorus is 0.0268C0(C0Initial melt concentration of gallium), preferably not more than 0.0326C0Over 0.0404C0A small part of inversion can occur; for antimony and boron compensated crystals, a suitable amount of borane to be doped is 0.0463C0(C0Initial melt concentration of antimony) ofPreferably more than 0.0569C0Over 0.0775C0A small fraction of inversion will occur. In practice the optimum gas doping level may vary within a range above and below the desired value.
In the manufacturing process of the czochralski silicon single crystal, polycrystalline silicon raw materials are placed in a quartz crucible, and a corresponding amount of solid phase dopant is added according to target resistivity, after the czochralski silicon is grown, the resistivity of the head part (the part where the crystal grows firstly) and the tail part (the part where the crystal grows and ends) of the crystal is different, so that the axial resistivity distribution is not uniform.
In order to improve the axial resistivity of the czochralski silicon single crystal, doping gas with the conductivity type opposite to that of the solid dopant is continuously and uniformly introduced in the constant-diameter growth stage of the czochralski silicon single crystal, after the constant-diameter growth is finished, the introduction of the doping gas is stopped, and the processes of ending, cooling and the like are continuously carried out under the protection of argon gas, so that the growth process of the whole silicon crystal is finished. The doping amount of the doping gas is 0.001-0.1 times of the initial melt concentration of the solid dopant. The specific value is calculated according to formula (3).
Preferably, when the solid dopant is gallium, the doping gas is phosphine, and the doping amount of the phosphine is 0.025-0.03 times of the initial melt concentration of the gallium.
The utilization rate of the produced czochralski silicon single crystal is close to 100 percent (the head and the tail of the crystal are removed), compared with 80 percent of czochralski silicon single crystal without doping gas, the utilization rate is obviously improved, and the resistivity of more than 90 percent of the area is controlled within the range of 0.5-3 omega.
Preferably, when the solid dopant is antimony, the doping gas is diborane, and the doping amount of the diborane is 0.045-0.055 time of the initial melt concentration of the antimony.
The axial resistivity variation of the produced Czochralski silicon single crystal in a region of 80% or more is controlled within a range of 25%.
Preferably, the doping gas in the step (3) is mixed with an inert gas.
The inert gas is used to dilute the dopant gas, and a gas that does not affect the crystal growth, such as argon, which is generally used as a protective gas for the crystal growth, or nitrogen, which is stable in properties, should be selected.
The mixed doping gas can be directly introduced into the crystal growth chamber, as shown in fig. 1, or the mixed doping gas can be introduced into the crystal growth chamber 6 through a high-purity quartz glass pipeline 7 after the mixed doping gas with a determined proportion is obtained by respectively arranging an inert gas source 2 and a doping gas source 4 and adjusting an inert gas flowmeter 1, a doping gas flowmeter 3 and a mixed gas flowmeter 5.
Preferably, the volume percentage of the inert gas in the doping gas is 1-99.9%. The volume percentage of the inert gas in the doping gas is not strictly limited, and the inert gas dilutes the doping gas, so that the inversion caused by the excessive local doping gas concentration in the czochralski silicon single crystal due to the excessive doping gas concentration is avoided.
Preferably, the flow rate of the doping gas introduced into the growth chamber is 1-1000 sccm (standard condition milliliters per minute).
The flow rate of the doping gas is determined according to the type and concentration of the doping gas and the type and concentration of the solid dopant in the crystal, the doping speed of the doping gas is required to be ensured to be adaptive to the growth speed of the crystal, the doping gas with opposite conductivity types is used for compensating the solid dopant, and the czochralski silicon single crystal with uniform axial resistivity is obtained.
The gallium-phosphorus-compensated Czochralski silicon for the solar cell prepared by the method for improving the uniformity of the axial resistivity of the Czochralski silicon has the axial resistivity of 0.5-3 omega cm in more than 90% of the area, and the antimony-boron-heavily-doped Czochralski silicon for the micro-electronics has the axial resistivity variation of less than 25% in more than 80% of the area.
The manufacturing method of the czochralski silicon provided by the invention has the following advantages:
(1) the type and the dosage of the doping gas are convenient to control, and various required impurity concentration distributions can be obtained;
(2) the utilization rate of the czochralski silicon single crystal is improved;
(3) the resistivity uniformity of the crystal is significantly improved.
Drawings
FIG. 1 is a schematic view of an apparatus for producing a Czochralski silicon single crystal by carrying out the method of the present invention;
FIG. 2 is a resistivity profile of a Czochralski silicon single crystal prepared in example 1;
FIG. 3 is a resistivity distribution diagram of a Czochralski silicon single crystal prepared in example 2.
Detailed Description
Example 1
60kg of high purity polysilicon feedstock was charged into a quartz crucible while 2.982g of high purity gallium (control head target resistivity 1.8 ohm. cm) was doped.
Under the protection of argon, the high-purity polysilicon is gradually heated to a temperature higher than 1420 ℃ so as to completely melt the high-purity polysilicon. Seeding and shouldering according to conventional crystal growth parameters, entering an equal-diameter growth stage, and controlling the crystal pulling rate to be 1.2mm/min and the crystal diameter to be 150 mm.
The furnace pressure was controlled at 20Torr and the argon flow was controlled at 70slpm (standard liters per minute).
Setting the parameters of the doping gas:
1) adopting phosphine diluted by argon as doping gas, wherein the volume ratio of the phosphine to the argon is 1: 1000;
2) assuming that the doping efficiency is 100% (the impurities introduced by the doping gas can be all introduced into the Czochralski silicon single crystal), the flow rate of the doping gas is set to 21.14 sccm.
And (4) closing the doping gas after the isometric growth is finished, normally ending, and cooling.
Samples were taken from different parts of the grown Czochralski silicon single crystal, and the resistivity distribution was measured using a four-probe resistivity meter, with the results shown in FIG. 2.
If the resistivity of the silicon wafer for the solar cell is controlled to be 0.5-3 ohm.cm, the utilization rate of the gallium-doped silicon single crystal is 75 percent; however, for the gallium and phosphorus co-doped single crystal silicon (i.e., the single crystal silicon into which the doping gas is introduced), the utilization rate can be increased to 93%, which means that the gallium and phosphorus co-doped single crystal silicon can be fully utilized after the head and tail portions are removed. Meanwhile, the resistivity distribution of the gallium-doped silicon single crystal is very uneven. For the gallium and phosphorus co-doped silicon single crystal, most of the resistivity is very uniform, the resistivity is reduced only in a very small part of the tail part, and the obtained silicon wafers can be used for preparing solar cells with high efficiency and no light attenuation.
Example 2
60kg of high purity polysilicon material was charged into a quartz crucible while 416.64g of high purity antimony (head target resistivity controlled to 0.016 ohm. cm) was doped.
Under the protection of argon, the polycrystalline silicon is heated to 1420 ℃ or higher gradually to be completely melted. Seeding and shouldering according to conventional crystal growth parameters, entering an equal-diameter growth stage, and controlling the crystal pulling rate to be 0.8mm/min and the crystal diameter to be 150 mm.
The furnace pressure was controlled at 20Torr and the argon flow was controlled at 70 slpm.
Setting the parameters of the doping gas:
1) adopting diborane diluted by argon, wherein the volume ratio of the diborane to the argon is 1: 100;
2) assuming a doping efficiency of 100%, the dopant gas flow rate was set to 97.58 sccm.
And after the isometric growth is finished, closing the doping gas, normally ending, and cooling.
Samples were taken from different parts of the grown single crystal silicon and the resistivity distribution was measured using a four-probe resistivity meter, the results of which are shown in FIG. 3.
If the requirement of a microelectronic manufacturer for 25% fluctuation of resistivity is met, the utilization rate of the antimony-doped monocrystalline silicon is only about 40%, and the utilization rate of the antimony-boron-codoped monocrystalline silicon (namely the monocrystalline silicon with doping gas introduced) can reach about 80%, which is increased by nearly 1 time, the utilization rate of the monocrystalline silicon is obviously improved, the resistivity uniformity is obviously improved, and the quality control of an integrated circuit is facilitated.
Claims (6)
1. A method for improving the uniformity of the axial resistivity of Czochralski silicon comprises melting a polycrystalline silicon raw material and a solid dopant in an argon atmosphere to obtain stable molten silicon; introducing seed crystals into the stable molten silicon, and leading the crystal growth to enter an isodiametric growth stage through necking and shouldering processes; the method is characterized in that doping gas with the conductivity type opposite to that of the solid dopant is introduced in the equal-diameter growth stage until the growth of the czochralski silicon is finished; the doping amount of the doping gas is 0.001-0.1 times of the initial melt concentration of the solid dopant.
2. The method of claim 1 wherein when the solid dopant is gallium, the dopant gas is phosphane in an amount of 0.025 to 0.03 times the initial melt concentration of gallium.
3. The method for improving the axial resistivity uniformity of czochralski silicon as claimed in claim 1, wherein when the solid dopant is antimony, the doping gas is diborane, and the doping amount of the diborane is 0.045-0.055 times of the initial melt concentration of the antimony.
4. The method for improving the axial resistivity uniformity of czochralski silicon as claimed in any one of claims 1 to 3, wherein an inert gas is mixed in the doping gas.
5. The method of improving the axial resistivity uniformity of czochralski silicon as claimed in claim 4 wherein the volume percent of inert gas in the dopant gas is 1 to 99.9%.
6. The method of improving the axial resistivity uniformity of czochralski silicon as claimed in claim 5, wherein the dopant gas is introduced into the growth chamber at a flow rate of 1 to 1000 sccm.
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| CN110158148A (en) * | 2019-04-29 | 2019-08-23 | 江苏协鑫软控设备科技发展有限公司 | Crystal silicon and its crystal growth technique |
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| CN114622278B (en) * | 2020-12-08 | 2024-04-05 | 内蒙古中环晶体材料有限公司 | Silicon single crystal and preparation method thereof, silicon wafer, solar cell and assembly |
| CN112831828B (en) * | 2021-01-07 | 2021-12-07 | 杭州晶宝新能源科技有限公司 | Growth method of gallium-doped Czochralski monocrystalline silicon, gallium-doped monocrystalline silicon and application |
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| CN102534752A (en) * | 2012-03-08 | 2012-07-04 | 天津市环欧半导体材料技术有限公司 | Czochralski zone melting gas doping method for preparing zone-melted silicon single crystal |
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