CN106012010A - Method and apparatus for secondary addition of doping agent - Google Patents
Method and apparatus for secondary addition of doping agent Download PDFInfo
- Publication number
- CN106012010A CN106012010A CN201610670967.XA CN201610670967A CN106012010A CN 106012010 A CN106012010 A CN 106012010A CN 201610670967 A CN201610670967 A CN 201610670967A CN 106012010 A CN106012010 A CN 106012010A
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- Prior art keywords
- doping agent
- feed bin
- silicon
- liquid
- secondary doping
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Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The invention relates to a method for secondary addition of a doping agent. The method comprises the following steps: fusing a silicon material containing the doping agent to silicon liquid; and growing crystal, wherein, during a crystal growth phase, the secondary doping agent is introduced into the silicon liquid as a liquid state. According to the above method, the doping agent is introduced into the silicon liquid as the liquid state, impact on fused silicon liquid level is reduced, and impurity generation probability is reduced. Through secondary addition of the doping agent, distribution of the silicon ingot-doped elements is improved, adverse resistivity is reduced, mechanical strength of a silicon chip is increased, and so that the ingot casting yield and silicon chip quality of a silicon ingot are increased. The invention also provides an apparatus for secondary addition of doping agent used for polycrystalline ingot casting production.
Description
Technical field
The present invention relates to solar energy photovoltaic material preparation field, the secondary being specifically related to a kind of crystal silicon ingot casting adds
The method and apparatus of adulterant.
Background technology
At present, crystal silicon solar batteries improved efficiency becomes one of key task of industry research.Wherein, fall
One of decay most efficient method becoming raising efficiency of the light of low crystal silicon solar batteries.The most conventional
Method is to substitute boron by gallium to prepare P-type silicon or by using N type dopant to prepare N-type crystalline silicon wafer.But
Gallium or the N type dopant segregation coefficient in silicon is smaller, and the resistivity that can cause crystal silicon permanent set is inclined
Low, thus affect the yield rate of silicon ingot, improve production cost.At present can be by during long crystalline substance
In silicon liquid, mix counter doping agent adjust resistivity, reduce production cost.But counter doping agent now is
Mix in silicon liquid with the form of solid-state, during mixing, liquid can be produced impact, cause solid-liquid circle
The stable state in face is destroyed, thus produces impurity shadow band, and affects yield.On the other hand, due to adulterant
Density more than molten silicon, cause the adulterant added in solid form to be positioned at solid-liquid long crystalline substance interface and assemble, expand
Dissipate uneven.
Summary of the invention
Based on this, it is necessary to provide a kind of method that secondary adds adulterant, it is possible to reduce mixing of secondary interpolation
The miscellaneous dose of impact to silicon liquid, reduces the probability producing shade impurity, improves ingot casting yield rate and Si wafer quality.
A kind of secondary adds the method for adulterant, including step:
It is silicon liquid by the melting silicon materials containing adulterant;
Long crystalline substance, in described crystal growing stage, makes secondary doping agent enter silicon liquid in the way of liquid.
Above-mentioned secondary adds the method for adulterant, secondary doping agent is added in the way of liquid in silicon liquid, subtracts
Lack the impact to fusion silicon liquid level, decrease the probability that impurity produces.And add adulterant by secondary, change
The distribution of kind silicon ingot doped chemical, reduces resistivity bad or promote the mechanical strength of silicon chip, thus promotes silicon
The ingot casting yield rate of ingot and Si wafer quality.
Wherein in an embodiment, described secondary doping agent is phosphorus, germanium, antimony, the simple substance of boron or alloy.
Wherein in an embodiment, described long crystalline substance, in described crystal growing stage, make secondary doping agent with liquid
The mode of state enters the step of silicon liquid and includes:
When crystal area proportion reaches predetermined value, control to drop to above silicon liquid equipped with the feed bin of described secondary doping agent;
Utilize the temperature above silicon liquid to make described secondary doping agent melt, then offer via described feed bin bottom
Discharging opening flow into described silicon liquid.
Wherein in an embodiment, the fusing point of described secondary doping agent is less than 1000 DEG C.
Wherein in an embodiment, described long crystalline substance, in described crystal growing stage, make secondary doping agent with liquid
The mode of state enters the step of silicon liquid and includes:
When crystal area proportion reaches predetermined value, control to drop to above silicon liquid equipped with the feed bin of described secondary doping agent;
The temperature of the heater promoting ingot furnace makes described secondary doping agent melt, at the bottom of then via described feed bin
The discharging opening that end is offered flows into described silicon liquid.
Wherein in an embodiment, the discharging opening of described feed bin and the distance of surface of the silicon liquid are 0~5 centimetre.
Wherein in an embodiment, in described crystal growing stage, secondary doping agent is made to enter in the way of liquid
The step entering silicon liquid includes:
When crystal area proportion reaches predetermined value, control to drop to above silicon liquid equipped with the feed bin of described secondary doping agent,
Utilization is arranged on secondary doping agent described in the heating element heats outside described feed bin makes described secondary doping agent melt
Changing, the discharging opening then offered via described feed bin bottom flows into described silicon liquid.
Also propose a kind of secondary and add the device of adulterant, including:
Feed bin, is used for holding secondary doping agent, and the bottom of described feed bin is provided with discharge opening;
Connecting rod, is connected with described feed bin, in order to drive described feed bin to lift.
Wherein in an embodiment, the outside of described feed bin is provided with heating element heater.
Wherein in an embodiment, the material of described feed bin is silicon nitride or quartz.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet that secondary of the present invention adds the method for adulterant;
Fig. 2 is the structural representation that secondary of the present invention adds the device of adulterant;
Fig. 3 is the enlarged drawing of X section in Fig. 2;
Fig. 4 is the schematic diagram that secondary of the present invention adds the device duty of adulterant.
Detailed description of the invention
Understandable for enabling the above-mentioned purpose of the present invention, feature and advantage to become apparent from, the most right
The detailed description of the invention of the present invention is described in detail.Elaborate in the following description a lot of detail with
It is easy to fully understand the present invention.But the present invention can come real to be a lot different from alternate manner described here
Executing, those skilled in the art can do similar improvement in the case of intension of the present invention, therefore this
Bright do not limited by following public specific embodiment.
Unless otherwise defined, all of technology used herein and scientific terminology and the technology belonging to the present invention
The implication that the technical staff in field is generally understood that is identical.The art used the most in the description of the invention
Language is intended merely to describe the purpose of specific embodiment, it is not intended that in limiting the present invention.Used herein
Term " and/or " include the arbitrary and all of combination of one or more relevant Listed Items.
Below in conjunction with the accompanying drawings, the better embodiment of the present invention is described.
The present invention provides a kind of method that secondary adds adulterant.Ginseng Fig. 1, the method includes:
Step S110, it is silicon liquid by the melting silicon materials containing adulterant.
In crucible, load silicon material, silicon material is mixed with adulterant, to control the target electricity of the crystal of primary crystallization
Resistance rate.Adulterant is N-type or the semiconductor element of p-type or foundry alloy.
Step S120, long crystalline substance, in described crystal growing stage, make secondary doping agent enter silicon in the way of liquid
Liquid.After melting silicon materials, control the temperature in ingot furnace, form thermograde from bottom to top, so that silicon liquid
Directional solidification, enters crystal growing stage.
In crystal growing stage, when crystal area proportion reaches predetermined value, fusing secondary doping agent becomes liquid,
Then enter in the way of liquid in silicon liquid.
The conduction type of secondary doping agent is contrary with the conduction type of the adulterant mixed in silicon material.Secondary doping
Agent is generally phosphorus, germanium, antimony, the simple substance of boron or alloy.
Silicon liquid can be entered in the way of liquid in several ways after making secondary doping agent fusing.
When mode one, crystal area proportion reach predetermined value, control to drop to equipped with the feed bin of described secondary doping agent
Above silicon liquid;The temperature above silicon liquid is utilized to make described secondary doping agent melt, then via on described feed bin
The discharging opening offered flows into described silicon liquid.
Secondary doping agent is contained in feed bin.When the fusing point of secondary doping agent is relatively small, such as secondary doping agent
Fusing point less than 1000 DEG C time, make feed bin drop to above silicon liquid, the discharging opening of feed bin distance surface of the silicon liquid 0~5
Centimetre.Owing to the fusing point of secondary doping agent is little, it is far below the temperature above silicon liquid, therefore utilizes above silicon liquid
Temperature described secondary doping agent can be made to melt, then flow into institute via the discharging opening offered on described feed bin
State silicon liquid.Depending on the opportunity of secondary doping agent fusing is according to wishing the target resistance values that crystal silicon reaches.
When mode two, crystal area proportion reach predetermined value, control to drop to equipped with the feed bin of described secondary doping agent
Above silicon liquid;The temperature of the heater promoting ingot furnace makes described secondary doping agent melt, then via described
The discharging opening offered on feed bin flows into described silicon liquid.
The discharging opening distance surface of the silicon liquid 0~5 centimetres of feed bin.Temperature above silicon liquid is not enough so that secondary is mixed
During miscellaneous dose of fusing, the temperature of the heater that can promote ingot furnace makes described secondary doping agent melt, then warp
Described silicon liquid is flowed into by the discharging opening offered on described feed bin.
When mode three, crystal area proportion reach predetermined value, control to drop to equipped with the feed bin of described secondary doping agent
Above silicon liquid, utilization is arranged on secondary doping agent described in the heating element heats outside described feed bin makes described two
Secondary adulterant melts, and then flows into described silicon liquid via the discharging opening offered on described feed bin.
The outside of feed bin can be independently arranged heating element heater.The discharging opening distance surface of the silicon liquid 0~5 lis of feed bin
Rice.When needing fusing, add heat fusing secondary doping agent by heating element heater, do not use and promote ingot furnace
The method of the temperature of heater, reduces the impact of thermal field in ingot furnace.
Secondary doping agent enters in silicon liquid in the way of liquid, thus decreases the impact to fusion silicon liquid level, subtracts
Lack the probability that impurity produces.And add adulterant by secondary, improve the distribution of silicon ingot doped chemical, fall
Low-resistivity is bad or promotes the mechanical strength of silicon chip, thus promotes ingot casting yield rate and the Si wafer quality of silicon ingot.
Ginseng Fig. 2 and Fig. 3, the device that the present invention adds adulterant for the secondary that ingot casting produces includes: feed bin
210 connecting rods 220 being connected with feed bin 210.
Feed bin 210 is used for holding secondary doping agent, and the bottom of feed bin 210 is provided with one or more, diameter
It it is the discharge opening 212 of 5~10 millimeters.The material of feed bin 210 is silicon nitride or quartz, to adapt to ingot furnace
High temperature.Ginseng Fig. 2, the inwall of feed bin 210 is provided with tapered portion.Discharge opening 212 is arranged on the top of tapered portion,
Consequently facilitating the secondary doping agent after Rong Hua flows out feed bin 212 through discharge opening 212 under gravity.
Connecting rod 220 is in order to drive feed bin 210 to lift, detachable fixing between itself and feed bin 210.
Such as can be fixed by snap, threaded, pin connects.The material of connecting rod 220 is nitridation
Silicon or quartz.
The outside of feed bin 210 can also arrange heating element heater.Heating element heater can be graphite heater or heating
Coil.Further, the outside of heating element heater can also include heat insulation felt, reduces and utilizes heating element heater to melt
Energy expenditure during secondary doping agent.
Fig. 4 illustrates the duty that secondary adds the device of adulterant.Secondary adds the device of adulterant to be put
Put in the guide shell 310 of ingot furnace 300 and can lift.During decline, secondary adds the device of adulterant
Can enter into above the silicon liquid 340 in crucible 330 through crucible cover plate 320.Secondary doping after fusing
Agent 400 can flow in silicon liquid in a liquid-like manner, thus reduces the impact to surface of the silicon liquid.
Below in conjunction with several embodiments introduce how during ingot casting secondary add adulterant.
Embodiment 1
Secondary doping agent 400 is placed in feed bin 210.The material of feed bin 210 is quartz material, wherein
The discharge opening 212 of a diameter of 5mm is had in the bottom of feed bin 210.Secondary doping agent 400 is antimony simple substance, weight
Amount is 4g.
Feed bin 210 is placed in guide shell 310 upper end.The polysilicon of 880kg is put in silica crucible 330,
Mix appropriate containing gallium foundry alloy (gallium concentration is 20000ppbw) simultaneously.Under argon gas atmosphere is protected,
1560 DEG C of melting polycrystalline silicon material and foundry alloy.Crystal growing stage is entered, when crystal growth crystallization ratio by normal process
When example reaches 75%, decline secondary doping device, make feed bin 210 be positioned at silicon liquid 340 surface.Due to
The fusion temperature of antimony is 630 DEG C of temperature well below melted silicon top, and antimony rapid melting, by feed bin 210
The discharge opening 212 of bottom enters in silicon liquid 340.It is promoted to lead by secondary doping device after standing a period of time
In flow cartridge 310.Continue long crystalline substance to terminating.After silicon ingot evolution, measure crystal resistivity by four probe method
Distribution, finds that the resistivity accounting for the silicon ingot of height 92% is all at 1~3 Ω cm.
The most cleaved formation of crystalline silicon silicon ingot that the method for resistivity is produced is controlled in crystalline silicon forming process
Silicon chip can be used to prepare efficient solaode.Due to can be by the crystalline silicon silicon ingot of the 90% of preparation
Resistivity controls in the range of 1.0~3.0 Ω cm, is conducive to increasing the utilization rate of silicon material, thus reduces
Production cost.The method is simple to operate, it is possible to achieve Automated condtrol, and beneficially photovoltaic industry on a large scale should
With.
Embodiment 2
Secondary doping agent 400 is placed in feed bin 210.The material of feed bin 210 is silicon nitride material, its
In have the discharge opening 212 totally 3 of a diameter of 5mm in the bottom of feed bin 210.Secondary doping agent 400 is germanium
Simple substance, weight is 500g.Feed bin 210 is placed in guide shell 310 upper end.The polysilicon of 880kg is put into
In silica crucible 330, mix appropriate boracic foundry alloy simultaneously.Under argon gas atmosphere is protected, at 1560 DEG C
Melting polycrystalline silicon material and foundry alloy.Crystal growing stage is entered, when crystal growth crystal area proportion reaches by normal process
When 20%, decline secondary doping device, owing to the fusion temperature of germanium is 937 DEG C, well below melted silicon top
Temperature, germanium rapid melting, entered in silicon liquid 340 by the discharge opening 212 of feed bin 210 bottom.Stand
After a period of time, secondary doping device is promoted in guide shell 310.Continue long crystalline substance to terminating.Germanium silicon will be mixed
After sheet is prepared as cell piece, testing efficiency finds improved efficiency 0.05%.
Embodiment 3
Secondary doping agent is placed in feed bin 210.The material of feed bin 210 is quartz material, wherein at material
There is the discharge opening 212 of a diameter of 10mm the bottom in storehouse 210.Outside feed bin 210 wrap up graphite heater and every
Hot felt.Secondary doping agent be doping content be 1019cm-3(wherein, 1019Represent atom number) boron-doping female
Alloy, weight is 78g.Feed bin 210 is placed in guide shell 310 upper end.The polysilicon of 880kg is put into stone
In English crucible 330, mix appropriate phosphorous foundry alloy (target resistivity is 2.8 Ω cm) simultaneously.At argon
Under atmosphere protection, at 1560 DEG C of melting polycrystalline silicon material and foundry alloy.Crystal growing stage is entered by normal process, when
When crystal growth crystal area proportion reaches 80%, graphite heater is heated to 1520 DEG C, makes temperature in feed bin 210
Raising, p-type foundry alloy gradually melts, and is entered in silicon liquid 340 by the discharge opening 212 of feed bin 210 bottom.
After standing a period of time, secondary doping device is promoted in guide shell 310.Continue long crystalline substance to terminating.Silicon ingot
After evolution, measured the distribution of crystal resistivity by four probe method, find to account for the resistance of the silicon ingot of height 86%
Rate, all at 1.5~2.5 Ω cm, accounts for the resistivity of silicon ingot of height 92% all at 1.0~3 Ω cm.
Each technical characteristic of embodiment described above can combine arbitrarily, for making description succinct, the most right
The all possible combination of each technical characteristic in above-described embodiment is all described, but, if these skills
There is not contradiction in the combination of art feature, is all considered to be the scope that this specification is recorded.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed,
But can not therefore be construed as limiting the scope of the patent.It should be pointed out that, for this area
For those of ordinary skill, without departing from the inventive concept of the premise, it is also possible to make some deformation and change
Entering, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be with appended power
Profit requires to be as the criterion.
Claims (10)
1. the method that a secondary adds adulterant, it is characterised in that include step:
It is silicon liquid by the melting silicon materials containing adulterant;
Long crystalline substance, in described crystal growing stage, makes secondary doping agent enter silicon liquid in the way of liquid.
Method the most according to claim 1, it is characterised in that described secondary doping agent be phosphorus, germanium,
Antimony, the simple substance of boron or alloy.
Method the most according to claim 1, it is characterised in that described long crystalline substance, in described crystal growing stage
In, the step making secondary doping agent enter silicon liquid in the way of liquid includes:
When crystal area proportion reaches predetermined value, control to drop to above silicon liquid equipped with the feed bin of described secondary doping agent;
Utilize the temperature above silicon liquid to make described secondary doping agent melt, then offer via described feed bin bottom
Discharging opening flow into described silicon liquid.
Method the most according to claim 3, it is characterised in that the fusing point of described secondary doping agent is less than
1000℃。
Method the most according to claim 1, it is characterised in that described long crystalline substance, in described crystal growing stage
In, the step making secondary doping agent enter silicon liquid in the way of liquid includes:
When crystal area proportion reaches predetermined value, control to drop to above silicon liquid equipped with the feed bin of described secondary doping agent;
The temperature of the heater promoting ingot furnace makes described secondary doping agent melt, at the bottom of then via described feed bin
The discharging opening that end is offered flows into described silicon liquid.
Method the most according to claim 1, it is characterised in that described long crystalline substance, in described crystal growing stage
In, the step making secondary doping agent enter silicon liquid in the way of liquid includes:
When crystal area proportion reaches predetermined value, control to drop to above silicon liquid equipped with the feed bin of described secondary doping agent,
Utilization is arranged on secondary doping agent described in the heating element heats outside described feed bin makes described secondary doping agent melt
Changing, the discharging opening then offered via described feed bin bottom flows into described silicon liquid.
7. according to the method described in any one of claim 2-6, it is characterised in that the discharging opening of described feed bin
It it is 0~5 centimetre with the distance of surface of the silicon liquid.
8. the device of a secondary interpolation adulterant, it is characterised in that including:
Feed bin, is used for holding secondary doping agent, and the bottom of described feed bin is provided with discharge opening;
Connecting rod, is connected with described feed bin, in order to drive described feed bin to lift.
Device the most according to claim 8, it is characterised in that the outside of described feed bin is provided with heating
Element.
Device the most according to claim 8, it is characterised in that the material of described feed bin is silicon nitride
Or quartz.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113668048A (en) * | 2021-08-20 | 2021-11-19 | 宁夏中欣晶圆半导体科技有限公司 | Low-resistivity heavily-doped phosphorus silicon single crystal production device and method |
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