CN102912424A - 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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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 present invention relates to field of semiconductor materials, be specifically related to a kind of method by the axial resistivity evenness of gas phase doping method raising pulling of silicon single crystal and the silicon single crystal that obtains.
Background technology
In a foreseeable future, photovoltaic generation is most important renewable energy technologies.According to EPIA (EPIA) prediction, the year two thousand thirty photovoltaic generation will satisfy the electricity needs in the whole world nearly 10%.
Present solar cell is based on mainly that the single crystal silicon material of boron-doping makes, but this battery is because contain simultaneously boron and oxygen in the silicon single crystal, in use can form boron oxygen complex body, cause the photoelectric transformation efficiency of solar cell to descend more than 10%, the performance of solar cell significantly reduces.For addressing this problem, the researchist has invented the single crystal silicon solar cell of mixing gallium.
Although mix the unglazed relaxation phenomenon of the single crystal silicon solar cell of gallium, but there is very large defective in it, because the segregation coefficient of gallium in silicon extremely low (approximately 0.008), this has just caused mixing in the gallium pulling of silicon single crystal process of growth, axially resistivity differs greatly, the resistivity of the silicon single crystal of last growth does not reach requirement in the pulling of silicon single crystal, only has about 80% so that mix the practical efficiency of gallium pulling of silicon single crystal.
In addition, the resistivity distribution of mixing the gallium pulling of silicon single crystal is wider, causes the efficiency distribution of solar cell also wide, has had a strong impact on the consistence of solar module power stage.
It is with high costs that these defectives cause mixing the gallium solar cell, meets difficulty in the industry member large-scale application.That up to the present, announces not yet both at home and abroad that a kind of effective means can obtain that axial uniform resistivity distributes mixes the gallium pulling of silicon single crystal.
At microelectronic, the reblended antimony pulling of silicon single crystal also is a kind of important materials, by its n/n+ epitaxial wafer of making have that zone of transition is narrow, the knot gradient is steep, the advantage such as the spread coefficient of antimony is little under the high temperature, make and mix antimony single crystal silicon and become a kind of important substrate.
But with gallium doped monocrystaline silicon similarly be, antimony is equilibrium segregation coefficient also very little (approximately 0.023) in silicon, and the axial resistivity evenness that causes equally mixing the antimony pulling of silicon single crystal is very poor.
Summary of the invention
The invention provides a kind of method that improves the axial resistivity evenness of pulling of silicon single crystal, by the method for gas phase doping, greatly improved the homogeneity of the axial resistivity of pulling of silicon single crystal, simple and practical, have good prospects for commercial application.
A kind of method that improves the axial resistivity evenness of pulling of silicon single crystal comprises the steps:
(1) melting under argon gas atmosphere with polycrystalline silicon raw material and solid dopants obtains stable molten silicon;
(2) introduce seed crystal in stable molten silicon, crystal is grown through necking down, shouldering process, enters the isodiametric growth stage;
(3) in the isodiametric growth stage, pass into the impurity gas with described solid dopants conductivity type opposite, until the pulling of crystals silicon growth is finished.
In the normal isodiametric growth process of czochralski silicon monocrystal, continue to pass into equably impurity gas and realize gas phase doping, following equation is obeyed in the distribution of gaseous impurities in silicon single-crystal that impurity gas is introduced:
Wherein,
C
sDoping content for the impurity in the silicon single-crystal;
A is the doping speed of impurity gas;
V is the growth velocity of pulling of silicon single crystal;
K is the segregation coefficient of the impurity of impurity gas introducing;
G is solid fraction.
If exist in the situation that p-type impurity and N-shaped impurity mixes altogether, following equation (mixing altogether as example take the gallium of p-type and the phosphorus of N-shaped) is obeyed in the distribution of current carrier in the silicon crystal:
Wherein,
P is the concentration of current carrier in the silicon crystal;
C
0Initial melt concentration for gallium;
k
1Segregation coefficient for gallium;
G is solid fraction;
A is the doping speed (impurity level of introducing in the unit time is by the flow control of impurity gas) of impurity gas;
V is the growth velocity of pulling of silicon single crystal;
k
2Segregation coefficient for phosphorus;
The impurity concentration that the expression impurity gas is introduced.
By regulating concentration and the flow of impurity gas, can obtain best gas phase doping amount, make the axial resistivity of czochralski silicon monocrystal keep evenly distributing.
Wherein best gas doping amount is:
Wherein,
C
0Initial melt concentration for solid dopants;
k
1Segregation coefficient for solid dopants;
A is the doping speed of impurity gas;
V is the growth velocity of pulling of silicon single crystal;
k
2Segregation coefficient for impurity in the impurity gas.
According to this formula, in the compensated crystal of gallium and phosphorus, the suitable doping of phosphine is 0.0268C
0(C
0Initial melt concentration for gallium), should not surpass 0.0326C
0, surpass 0.0404C
0The small part transoid can appear; For antimony and boron compensation crystal, the suitable doping of borine is 0.0463C
0(C
0Initial melt concentration for antimony), should not surpass 0.0569C
0, surpass 0.0775C
0The small part transoid can appear.In fact the optimal gas doping can change in the next scope on Appropriate.
In the czochralski silicon monocrystal manufacturing processed, polycrystalline silicon raw material is placed quartz crucible, drop into the solid phase doping agent of respective amount according to target resistivity, after the pulling of crystals silicon growth is finished, the resistivity of its crystal head (position of crystal grow first) and afterbody (position of crystal growth ending) can be variant, causes axial resistivity distribution inhomogeneous.
In order to improve the axial resistivity of czochralski silicon monocrystal; in the czochralski silicon monocrystal isodiametric growth stage; continue to pass into evenly the impurity gas with the solid dopants conductivity type opposite; after isodiametric growth finishes; stop to pass into impurity gas; continuation finishes up under the protection of argon gas and the process such as cooling, finishes the process of growth of whole silicon crystal.The doping of described impurity gas is 0.001～0.1 times of initial melt concentration of solid dopants.Concrete value calculates according to formula (3).
As preferably, when described solid dopants was gallium, described impurity gas was phosphine, and the doping of phosphine is 0.025～0.03 times of initial melt concentration of gallium.
The czochralski silicon monocrystal utilization ratio that produces is near 100% (removing crystal head and afterbody), compares the 80% czochralski silicon monocrystal utilization ratio that does not have impurity gas and has and significantly improve, and the resistivity in zone is controlled in 0.5～3 Ω .cm scope more than 90%.
As preferably, when described solid dopants was antimony, described impurity gas was diborane, and the doping of diborane is 0.045～0.055 times of initial melt concentration of antimony.
The axial change in resistance in the czochralski silicon monocrystal that produces zone more than 80% is controlled in 25% the scope.
As preferably, be mixed with rare gas element in the impurity gas in the described step (3).
Rare gas element is used for dopingtank gas, should select the gas that does not affect the crystal growth, for example generally is used as the argon gas of crystal growth protecting gas, perhaps the nitrogen of stable in properties.
The impurity gas that can directly mixing be finished passes in the crystal growing chamber, as shown in Figure 1, also can be by rare gas element source of the gas 2 and impurity gas source of the gas 4 be set respectively, by regulating the under meter 5 of rare gas element gas meter 1, dopant gas flow meter 3 and mixed gas, after obtaining determining the mixed gas of ratio, by purity quartz glass pipe for high road 7, pass in the crystal growing chamber 6.
As preferably, the percent by volume of rare gas element is 1～99.9% in the described impurity gas.The not strict restriction of the volume percent of rare gas element in the impurity gas, rare gas element dilutes impurity gas, has avoided the impurity gas excessive concentration, in the czochralski silicon monocrystal that may cause because of the excessive transoid that causes of local impurity gas concentration.
As preferably, the flow that described impurity gas passes into the growth room is 1～1000sccm (mark condition milliliter per minute).
The flow of impurity gas is according to the kind of solid dopants in kind, concentration and the crystal of impurity gas, concentration and decide, need to guarantee that the speed of mixing of impurity gas and the speed of growth of crystal adapt, the impurity gas of conductivity type opposite is compensated the solid phase doping agent, obtain the czochralski silicon monocrystal of axial uniform resistivity.
The axial resistivity in zone 90% or more of the gallium phosphorus compensation pulling of silicon single crystal that the solar cell that utilizes the method for the axial resistivity evenness of raising pulling of silicon single crystal of the present invention to prepare is used is 0.5～3 Ω cm, and the regional axial change in resistance more than 80% of the reblended antimony boron compensation pulling of silicon single crystal that microelectronics is used is less than 25%.
Pulling of silicon single crystal manufacture method provided by the invention has the following advantages:
(1) the convenient control of the kind of impurity gas and consumption can obtain various required impurities concentration distribution;
(2) improved the utilization ratio of czochralski silicon monocrystal;
(3) significantly improve the resistivity evenness of crystal.
Description of drawings
Fig. 1 makes the device schematic diagram of czochralski silicon monocrystal for implementing the inventive method;
Fig. 2 is the czochralski silicon monocrystal resistivity distribution figure that embodiment 1 prepares;
Fig. 3 is the czochralski silicon monocrystal resistivity distribution figure that embodiment 2 prepares.
Embodiment
The high-purity polycrystalline silicon raw material that in quartz crucible, adds 60kg, mix simultaneously 2.982g high purity gallium (control head target resistivity is 1.8 ohm. centimetre).
Under argon shield, heat to gradually more than 1420 ℃ high purity polycrystalline silicon is melted fully.According to conventional crystal growth parameter(s) seeding, shouldering, enter the isodiametric growth stage, control pulling rate 1.2mm/min, crystal diameter is 150mm.
Control furnace pressure 20Torr, argon flow amount is 70slpm (standard liters per minute).
Set the parameter of impurity gas:
1) phosphine that adopts argon-dilution is as impurity gas, the volume ratio of phosphine and argon gas 1: 1000;
2) suppose doping efficiency 100% (impurity of impurity gas introducing can all enter in the czochralski silicon monocrystal), setting the doping airshed is 21.14sccm.
Isodiametric growth is closed impurity gas after finishing, normal ending, cooling.
Finish the czochralski silicon monocrystal different sites sampling of growth, using four point probe resistivity meter test resistance rate to distribute, the result as shown in Figure 2.
If be controlled at 0.5～3 ohm according to solar cell with silicon chip resistivity. centimetre requirement, the silicon single-crystal utilization ratio of only mixing gallium is 75%; But for gallium and phosphor codoping silicon single crystal (namely passing into the silicon single crystal of impurity gas), its utilization ratio can be increased to 93%, and after this meaning was removed head and afterbody, the silicon single crystal of gallium phosphor codoping can access whole utilizations.Simultaneously, only its resistivity distribution of gallium-mixing silicon monocrystal is very inhomogeneous.And for the silicon single-crystal of gallium and phosphor codoping, its most of resistivity is very even, only descend to some extent in afterbody small part resistivity, and these silicon chips that obtain can both prepare high-level efficiency, the solar cell of unglazed decay.
The high-purity polycrystalline silicon raw material that in quartz crucible, adds 60kg, mix simultaneously 416.64g high purity antimony (control head target resistivity is 0.016 ohm. centimetre).
Under argon shield, heat to gradually more than 1420 ℃ polysilicon is melted fully.According to conventional crystal growth parameter(s) seeding, shouldering, enter the isodiametric growth stage, control pulling rate 0.8mm/min, crystal diameter is 150mm.
Control furnace pressure 20Torr, argon flow amount is 70slpm.
Set the parameter of impurity gas:
1) diborane of employing argon-dilution, the volume ratio of diborane and argon gas 1: 100;
2) suppose doping efficiency 100%, setting the doping airshed is 97.58sccm.
Isodiametric growth is closed impurity gas after finishing, normal ending, cooling.
Finish the silicon single crystal different sites sampling of growth, using four point probe resistivity meter test resistance rate to distribute, the result as shown in Figure 3.
If according to the requirement of microelectronics manufacturer to change in resistance unsteady 25%, for the silicon single crystal of only mixing antimony, utilization ratio only is about 40%, and the silicon single crystal (namely having passed into the silicon single crystal of impurity gas) of mixing altogether for antimony boron, utilization ratio can reach about 80%, has increased nearly 1 times, has improved significantly the utilization ratio of silicon single crystal, and significantly improved resistivity evenness, the quality control that utilizes unicircuit has been arranged.
Claims (9)
1. a method that improves the axial resistivity evenness of pulling of silicon single crystal comprises the melting under argon gas atmosphere with polycrystalline silicon raw material and solid dopants, obtains stable molten silicon; Introduce seed crystal in stable molten silicon, crystal is grown through necking down, shouldering process, enters the isodiametric growth stage; It is characterized in that, in the isodiametric growth stage, pass into the impurity gas with described solid dopants conductivity type opposite, until the pulling of crystals silicon growth is finished.
2. the method for the axial resistivity evenness of raising pulling of silicon single crystal as claimed in claim 1 is characterized in that, the doping of described impurity gas is 0.001～0.1 times of initial melt concentration of solid dopants.
3. the method for the axial resistivity evenness of raising pulling of silicon single crystal as claimed in claim 2 is characterized in that, when described solid dopants was gallium, described impurity gas was phosphine, and the doping of phosphine is 0.025～0.03 times of initial melt concentration of gallium.
4. the method for the axial resistivity evenness of raising pulling of silicon single crystal as claimed in claim 2 is characterized in that, when described solid dopants was antimony, described impurity gas was diborane, and the doping of diborane is 0.045～0.055 times of initial melt concentration of antimony.
5. such as the method for the axial resistivity evenness of the arbitrary described raising pulling of silicon single crystal of claim 1～4, it is characterized in that, be mixed with rare gas element in the impurity gas in the described step (3).
6. the method for the axial resistivity evenness of raising pulling of silicon single crystal as claimed in claim 5 is characterized in that, the percent by volume of rare gas element is 1～99.9% in the described impurity gas.
7. the method for the axial resistivity evenness of raising pulling of silicon single crystal as claimed in claim 6 is characterized in that, the flow that described impurity gas passes into the growth room is 1～1000sccm.
8. the pulling of silicon single crystal for preparing of the method for the axial resistivity evenness of raising pulling of silicon single crystal as claimed in claim 3 is characterized in that, the axial resistivity in zone is 0.5～3 Ω cm more than 90%.
9. the pulling of silicon single crystal for preparing of the method for the axial resistivity evenness of raising pulling of silicon single crystal as claimed in claim 4 is characterized in that, the axial change in resistance in zone is less than 25% more than 80%.
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| CN114540950A (en) * | 2022-01-10 | 2022-05-27 | 浙江大学 | Method for growing n-type czochralski silicon by reducing furnace pressure |
| CN116288658A (en) * | 2023-05-22 | 2023-06-23 | 苏州晨晖智能设备有限公司 | Single crystal furnace with intermittent doping at top and doping method thereof |
| CN116288658B (en) * | 2023-05-22 | 2023-10-24 | 苏州晨晖智能设备有限公司 | Single crystal furnace with intermittent doping at top and doping method thereof |
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