CN102534753A - Czochralski zone melting gas doping method for effectively improving radial resistivity uniformity of zone-melted silicon single crystal - Google Patents
Czochralski zone melting gas doping method for effectively improving radial resistivity uniformity of zone-melted silicon single crystal Download PDFInfo
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- CN102534753A CN102534753A CN2012100597564A CN201210059756A CN102534753A CN 102534753 A CN102534753 A CN 102534753A CN 2012100597564 A CN2012100597564 A CN 2012100597564A CN 201210059756 A CN201210059756 A CN 201210059756A CN 102534753 A CN102534753 A CN 102534753A
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Abstract
The invention relates to a Czochralski zone melting gas doping method for effectively improving the radial resistivity uniformity of a zone-melted silicon single crystal. During the production of a polycrystalline silicon rod, polycrystalline silicon with consistent axial resistivity is obtained by a double quartz crucible method and a decompression Czochralski method, is machined and annealed, and is put into a zone melting furnace, and the single crystal is pulled by a zone melting method; and if the target concentration of a dopant of the zone-melted silicon single crystal is c0, the concentration of the dopant at the tail of the polycrystalline silicon is controlled to be c0, wherein k is the segregation coefficient of the dopant. The concentration of the dopant of the polycrystalline rod is uniform, and gas doping is not required to be performed at a retention stage, so the concentration uniformity of a silicon melt is extremely high. Therefore, compared with a neutron transmutation doping (NTD) method, the method is low in cost and short in production period; and compared with a zone melting gas doping method and a Czochralski zone melting method, the method has the advantage that: the radial resistivity uniformity is effectively improved.
Description
Technical field
The present invention relates to the method for a kind of production area silicon crystal, the particularly a kind of effective raising zone-melted silicon single crystal radially molten gas in vertical pulling district of resistivity evenness is mixed method.
Background technology
Production extrinsic region silicon crystal prior art mainly contains: NTD method, the molten gas in district are mixed three kinds of method and vertical pulling and zone melting process.
The zone-melted silicon single crystal resistivity evenness that NTD neutron irradiation method is produced is the highest, but cost is bigger, and the production cycle is long.
Qu Rong gas is mixed method in process of production, through feeding the gaseous state doping agent zone-melted silicon single crystal is mixed.The gaseous state doping agent is incorporated into doping agent in the silicon melt through gas liquid film, and then behind the silicon melt solidification and crystallization, successfully doping agent is mixed in the silicon single-crystal.Can know that through the doping agent mobile route concentration of dopant of bath surface is higher, and the inner concentration of dopant of melt is lower.And because in the zone melting method, the volume of silicon melt is less, a little less than the convection current, to the stirring action of doping agent very a little less than, finally cause in the zone-melted silicon single crystal dopant distribution uneven, this also is to cause the radially uneven one of the main reasons of resistivity of zone-melted silicon single crystal.
Vertical pulling and zone melting process at first adopts vertical pulling method to draw the policrystalline silicon rod, and doping agent was incorporated in the polycrystalline silicon rod through conventional doping way in the vertical pulling stage.Along with the continuous solidification and crystallization of silicon melt, receive the influence of segregation effect, concentration of dopant is also increasingly high in the silicon melt, and the silicon crystal resistivity of solidifying is also more and more lower.Again because silicon crystal bar center heat radiation is slow, the edge rapid heat dissipation, thereby its solid-liquid interface is last spill, in polycrystalline silicon rod, can form the constant resistance rate face of spill like this, and resistivity reduces gradually.
Draw the stage at zone melting method, if the polycrystalline silicon rod head is downward, on the change material interface of polycrystalline silicon rod, the silicon melt resistivity of fusing is comparatively approaching, and the silicon melt resistivity that then provides for silicon monocrystal growth is comparatively even.But because the axial resistivity of polycrystalline silicon rod itself is inhomogeneous, add the influence of segregation effect, the axial resistivity gradient of the zone-melted silicon single crystal of drawing is very big.Equally, zone-melted silicon single crystal center heat radiation is slow, the edge rapid heat dissipation, and its solid-liquid interface is spill down, so the constant resistance rate face of zone-melted silicon single crystal is spill down.Bigger axial resistivity gradient causes silicon chip center resistivity and edge resistivity to differ bigger, thereby greatly reduces the radially resistivity evenness of zone-melted silicon single crystal.
Draw the stage at zone melting method; If the polycrystalline silicon rod head upwards; Because the influence of the axial resistivity distribution of policrystalline silicon itself and the influence of segregation phenomena though the axial resistivity distribution of the zone-melted silicon single crystal that is drawn makes moderate progress when more downward than head, still can not be effectively controlled.Secondly polycrystalline silicon rod melts the silicon melt of fusing at the interface, and its resistivity difference is bigger, can not obtain under effective melt convection effect, and melt resistivity is comparatively inhomogeneous, has finally also reduced the radially resistivity evenness of zone-melted silicon single crystal.
Summary of the invention
The object of the invention is exactly for overcoming the deficiency of prior art, the radially vertical pulling and zone melting process of resistivity evenness of a kind of effective raising zone-melted silicon single crystal is provided, compare the method with NTD, and cost is lower, and the production cycle is shorter; Compare with vertical pulling and zone melting process with the molten gas method of mixing in district, radially resistivity evenness has obtained effective raising.
The present invention realizes through such technical scheme: a kind of effective raising zone-melted silicon single crystal radially molten gas in vertical pulling district of resistivity evenness is mixed method; It is characterized in that; When the production of policrystalline silicon rod, adopt biquartz crucible method, step-down vertical pulling method to obtain axially and the consistent policrystalline silicon of resistivity radially, afterwards policrystalline silicon is carried out machining and anneals being placed in the zone melting furnace; Carry out crystal-pulling through zone melting method; If zone melting single-crystal silicon dopant aimed concn is c0, the afterbody concentration of dopant of then controlling policrystalline silicon is c0, and k is the doping agent segregation coefficient; Said method comprises the steps:
1) adopts biquartz crucible vertical pulling method to draw polycrystalline silicon rod, make the whole excellent concentration of polysilicon be c0, polycrystalline silicon rod is carried out barreling, fluting and reduction machining;
2) polysilicon after the employing machining adopts zone melting method to carry out crystal pulling as raw material, when crystal pulling is melted in the district, from expanding the shoulder stage, feeds quantitative doping gas, and doping gas can be phosphine or borine; When doping gas was phosphine, concentration of dopant reached value c0/k=1.7 * 10 in the silicon melt
14Atom/cm
3To 6.5 * 10
21Atom/cm
3Promptly stop to feed doping gas after the scope; When doping gas was borine, concentration of dopant reached value c0/k=7.6 * 10 in the silicon melt
13To 1.6 * 10
21Atom/cm
3Promptly stop to feed doping gas after the scope;
3) the maintenance stage, suppose that crystalline volume is V0, the new melt volume that then flows into is V0, the silicon melt constant volume is constant; Because crystalline monocrystalline concentration is c0, then silicon melt doping agent reduction is c0*V0, and the doping agent that increases newly is c0*V0, and the doping agent total amount is constant, and final silicon melt concentration of dopant maintains c0/k, and the concentration of silicon single-crystal also is stabilized in the c0 target value;
The zone-melted silicon single crystal for preparing according to above-mentioned steps radially resistivity evenness reach＜7%.
The invention has the beneficial effects as follows: because the concentration of dopant uniformity of polycrystalline charge bar of the present invention, and the maintenance stage need not to carry out gas and mix, then silicon melt concentration homogeneity is very high; In sum; The present invention compares the method with NTD, and cost is lower, and the production cycle is shorter; Compare with vertical pulling and zone melting process with the molten gas method of mixing in district, radially resistivity evenness has obtained effective raising.
Description of drawings
Fig. 1 is a vertical pulling and zone melting process crystal pulling synoptic diagram;
Fig. 2 is a vertical pulling and zone melting process, crystal pulling synoptic diagram when vertical pulling polycrystalline head is downward;
Fig. 3 is a vertical pulling and zone melting process, crystal pulling synoptic diagram when vertical pulling polycrystalline head makes progress;
Fig. 4 draws the polycrystalline synoptic diagram for vertical pulling method.
Wherein 1 is the polycrystalline charge bar, and 2 is silicon melt, and 3 are the molten polycrystalline in district, and 4 are polycrystalline fusing face, and 5 is vertical pulling polycrystalline charge bar constant resistance rate line.
Embodiment
As shown in Figures 1 to 4, adopt two crucible methods or step-down vertical pulling method to draw the consistent policrystalline silicon rod of radial and axial resistivity distribution, and concentration of dopant is c0.
201110092539.0), step-down vertical pulling method (number of patent application: 201110084578.6), obtain the consistent policrystalline silicon of axial resistivity when the production of policrystalline silicon rod, adopt biquartz crucible method (number of patent application:.Afterwards policrystalline silicon is carried out machining and anneal being placed in the zone melting furnace, carry out crystal-pulling through zone melting method.
Polycrystalline rod is carried out barreling, and after the machinings such as cutting, sharpening, its thermal stresses and mechanical workout stress are eliminated in annealing.
Polycrystalline silicon rod is placed in the zone melting furnace preheating, change material, and beginning crystal pulling.
Behind seeding, the drawing-down neck; Reduce lower shaft speed and begin to expand shoulder, in expanding the shoulder process and isometrical maintenance initial stage feeding impurity gas, make that concentration of dopant is c0/k in the silicon melt with the lower shaft rotating speed; Stop to feed doping gas after the isometrical maintenance, can guarantee that like this silicon single-crystal concentration of dopant is c0.
According to above-mentioned explanation, can realize scheme of the present invention in conjunction with art technology.
Claims (1)
- One kind effectively improve zone-melted silicon single crystal radially the molten gas in vertical pulling district of resistivity evenness mix method, it is characterized in that, when the production of policrystalline silicon rod; Adopt biquartz crucible method, step-down vertical pulling method to obtain axially and the consistent policrystalline silicon of resistivity radially; Afterwards policrystalline silicon is carried out machining and anneal being placed in the zone melting furnace, carry out crystal-pulling through zone melting method, if zone melting single-crystal silicon dopant aimed concn is c0; The afterbody concentration of dopant of then controlling policrystalline silicon is c0, and k is the doping agent segregation coefficient; Said method comprises the steps:1) adopts biquartz crucible vertical pulling method to draw polycrystalline silicon rod, make the whole excellent concentration of polysilicon be c0, polycrystalline silicon rod is carried out barreling, fluting and reduction machining;2) polysilicon after the employing machining adopts zone melting method to carry out crystal pulling as raw material, when crystal pulling is melted in the district, from expanding the shoulder stage, feeds quantitative doping gas, and doping gas can be phosphine or borine; When doping gas was phosphine, concentration of dopant reached value c0/k=1.7 * 10 in the silicon melt 14Atom/cm 3To 6.5 * 10 21Atom/cm 3Promptly stop to feed doping gas after the scope; When doping gas was borine, concentration of dopant reached value c0/k=7.6 * 10 in the silicon melt 13To 1.6 * 10 21Atom/cm 3Promptly stop to feed doping gas after the scope;3) the maintenance stage, suppose that crystalline volume is V0, the new melt volume that then flows into is V0, the silicon melt constant volume is constant; Because crystalline monocrystalline concentration is c0, then silicon melt doping agent reduction is c0*V0, and the doping agent that increases newly is c0*V0, and the doping agent total amount is constant, and final silicon melt concentration of dopant maintains c0/k, and the concentration of silicon single-crystal also is stabilized in the c0 target value;The zone-melted silicon single crystal for preparing according to above-mentioned steps radially resistivity evenness reach＜7%.
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| CN103866376A (en) * | 2012-12-13 | 2014-06-18 | 有研半导体材料股份有限公司 | Technical method for drawing high-resistivity zone-melting single crystal silicon with diameter of 80mm |
| TWI620839B (en) * | 2015-08-26 | 2018-04-11 | 中美矽晶製品股份有限公司 | Polycrystalline silicon column and polycrystalline silicon wafer |
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Application publication date: 20120704 |