CN109137068A - A kind of method for annealing of monocrystalline silicon piece - Google Patents
A kind of method for annealing of monocrystalline silicon piece Download PDFInfo
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- CN109137068A CN109137068A CN201810899888.5A CN201810899888A CN109137068A CN 109137068 A CN109137068 A CN 109137068A CN 201810899888 A CN201810899888 A CN 201810899888A CN 109137068 A CN109137068 A CN 109137068A
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- 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
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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
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Abstract
The invention discloses a kind of method for annealing of monocrystalline silicon piece.Include: a, starting annealing furnace, and be filled with protective gas, temperature is risen to 740~760 DEG C, 25~35 minutes is kept the temperature, is put into monocrystalline silicon piece, again at 740~760 DEG C, keeps the temperature 10~40 minutes；B, the temperature of annealing furnace is down to 640~660 DEG C, keeps the temperature 10~40 minutes；C, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is put into Feng Lin mechanism, a Lateral supply, one side air-out, air outlet is equipped with condensation unit and cools down to air inlet, cold air is blowed to monocrystalline silicon piece by blower, wind speed is 3~7m/s, air themperature is 10~16 DEG C, monocrystalline silicon piece is placed on intermediate air duct, and cold wind is allowed to blow over lower planes from side, guarantees that two sides are uniform, in 3~5min, monocrystalline silicon piece is cooled to room temperature.The beneficial effects of the present invention are: the phenomenon that capable of effectively eliminating the resistivity virtual height as caused by oxygen alms giver's effect, the resistance value after annealing is stablized, and it is small to float.
Description
Technical field
The present invention relates to monocrystalline silicon fields, and in particular to a kind of method for annealing of monocrystalline silicon piece.
Background technique
15 inches of monocrystalline silicon belong to large-diameter monocrystalline silicon product, and growth technique has harsh requirement, but is using
During vertical pulling method is grown, since silica crucible to be used is as container, the main material of silica crucible is quartz
SiO2, the oxygen atom of the inside can enter in silicon liquid over time, and refer to during the growth process to the inherence of crystal
Mark has an impact.Wherein a kind of most important influence is that the resistivity of crystal is caused to get higher.In the mistake of 15 inches of monocrystalline silicon growings
Cheng Zhong, oxygen are easily accumulated on crystals, form oxygen alms giver, lead to the resistivity virtual height of crystals, in particular for height
The silicon rod of resistivity.It can not check the inside true resistance rate value of crystal.It can usually be eliminated by annealing process
Oxygen alms giver's phenomenon of crystals, is directed to silicon for solar cell stick and silicon wafer, can be easy to eliminate oxygen alms giver, but
It is to be directed to major diameter single crystal, since its area is big, with the thickness of a bit, can deposits after annealing, sheet resistance is unevenly distributed
It is even, influence the final result of resistivity.
The annealing object of this technique is 15 inches of diameter, the disk of thickness 10mm.Because monocrystalline silicon piece size is larger, heat
Heating power distribution in monocrystalline silicon sheet surface and inside is uneven.Therefore removal is only reached by effectively annealing process
Oxygen alms giver's effect obtains the purpose that crystal is really resistivity.Using common annealing process, that is, it is placed on annealing furnace high-temperature
After 650 DEG C, heat preservation 30 minutes, natural cooling is carried out, requirement is unable to reach.
Diameter is greater than 385mm, and thickness is greater than 10mm monocrystalline monocrystalline silicon piece because diameter and thickness is bigger than normal, in annealing process
There are oxygen alms giver eliminate it is insufficient, often there is the phenomenon that secondary oxidation, directly affect resistivity measurement, cause detection data not
Stablize.
In order to solve the annealing problems of this type monocrystalline silicon piece, spy has developed targeted annealing process.
Summary of the invention
The purpose of the present invention is to provide a kind of method for annealing of monocrystalline silicon piece, can reduce resistance value, and it is floating to reduce resistance value
It is dynamic.
To achieve the above object, the present invention adopts the following technical scheme that, a kind of method for annealing of monocrystalline silicon piece, comprising:
A, start annealing furnace, and be filled with protective gas, temperature is risen to 740~760 DEG C, 25~35 minutes is kept the temperature, is put into
Monocrystalline silicon piece keeps the temperature 10~40 minutes again at 740~760 DEG C；
B, the temperature of annealing furnace is down to 640~660 DEG C, keeps the temperature 10~40 minutes；
C, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is put into Feng Lin mechanism, a Lateral supply a, side air-out is sent
Air port is equipped with condensation unit and cools down to air inlet, cold air is blowed to monocrystalline silicon piece by blower, wind speed is 3~7m/s, air themperature
It is 10~16 DEG C, monocrystalline silicon piece is placed on intermediate air duct, and cold wind is allowed to blow over lower planes from side, guarantees two sides
Uniformly, in 3~5min, monocrystalline silicon piece is cooled to room temperature；
Wherein, in step c, temperature lowering curve function are as follows:
T is rate of temperature fall DEG C/s, and t is the time s of cooling, and v is wind speed m/s, and C is the specific heat capacity C=of monocrystalline silicon
0.219cal/gk, R are the density 2.33g/cm of monocrystalline silicon for the thickness cm, ρ that the radius cm, H of monocrystalline silicon are silicon wafer3。
Preferably, the protective gas described in step a is argon gas.
Preferably, after monocrystalline silicon piece is put into step a at 750 DEG C, keep the temperature 30 minutes.
Preferably, in stepb, the temperature of annealing furnace is down to 650 DEG C, keeps the temperature 30 minutes.
Preferably, in step c, wind speed 4m/s, air themperature is 14 DEG C.
Preferably, the monocrystalline silicon piece should be pre-processed before step a, the pretreated method is by monocrystalline
Silicon is put into the mixed solution of hydrofluoric acid, ethyl alcohol and deionized water and cleans, then with being dried with nitrogen；Occlusion body in the mixed solution
The hydrofluoric acid that fraction is 5~10%, 10~20% ethyl alcohol, remaining is deionized water.
The beneficial effects of the present invention are: showing for the resistivity virtual height as caused by oxygen alms giver's effect can effectively be eliminated
As the resistance value after annealing is stablized, and it is small to float.
Specific embodiment
Invention is described in further detail below, to enable those skilled in the art's refer to the instruction text can be accordingly
Implement.
Embodiment 1
A, monocrystalline silicon is put into the mixed solution of hydrofluoric acid, ethyl alcohol and deionized water and is cleaned, then with being dried with nitrogen；It is described
The hydrofluoric acid for being 8% comprising volume fraction in mixed solution, 15% ethyl alcohol, remaining is deionized water；
B, start annealing furnace, and be filled with protective gas, temperature is risen to 750 DEG C, 30 minutes is kept the temperature, is put into monocrystalline silicon piece,
Again at 750 DEG C, 30 minutes are kept the temperature；
C, the temperature of annealing furnace is down to 650 DEG C, keeps the temperature 30 minutes；
D, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is put into Feng Lin mechanism, a Lateral supply a, side air-out is sent
Air port is equipped with condensation unit and cools down to air inlet, and cold air is blowed to monocrystalline silicon piece, wind speed 4m/s, air themperature 14 by blower
DEG C, monocrystalline silicon piece is placed on intermediate air duct, and cold wind is allowed to blow over lower planes from side, guarantees that two sides are uniform,
In 4min, monocrystalline silicon piece is cooled to room temperature；Temperature lowering curve function are as follows:T
It is the time s of cooling for rate of temperature fall DEG C/s, t, v is wind speed m/s, and C is specific heat capacity=0.219cal/gk of monocrystalline silicon, and R is
The radius cm, H of monocrystalline silicon are that the thickness cm, ρ of silicon wafer are the density 2.33g/cm of monocrystalline silicon3。
Embodiment 2
A, monocrystalline silicon is put into the mixed solution of hydrofluoric acid, ethyl alcohol and deionized water and is cleaned, then with being dried with nitrogen；It is described
The hydrofluoric acid for being 5% comprising volume fraction in mixed solution, 20% ethyl alcohol, remaining is deionized water；
B, start annealing furnace, and be filled with protective gas, temperature is risen to 740 DEG C, 35 minutes is kept the temperature, is put into monocrystalline silicon piece,
Again at 740 DEG C, 40 minutes are kept the temperature；
C, the temperature of annealing furnace is down to 640 DEG C, keeps the temperature 40 minutes；
D, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is put into Feng Lin mechanism, a Lateral supply a, side air-out is sent
Air port is equipped with condensation unit and cools down to air inlet, and cold air is blowed to monocrystalline silicon piece, wind speed 3m/s, air themperature 16 by blower
DEG C, monocrystalline silicon piece is placed on intermediate air duct, and cold wind is allowed to blow over lower planes from side, guarantees that two sides are uniform,
In 3min, monocrystalline silicon piece is cooled to room temperature；Temperature lowering curve function are as follows:T
It is the time s of cooling for rate of temperature fall DEG C/s, t, v is wind speed m/s, and C is specific heat capacity=0.219cal/gk of monocrystalline silicon, and R is
The radius cm, H of monocrystalline silicon are that the thickness cm, ρ of silicon wafer are the density 2.33g/cm of monocrystalline silicon3。
Embodiment 3
A, monocrystalline silicon is put into the mixed solution of hydrofluoric acid, ethyl alcohol and deionized water and is cleaned, then with being dried with nitrogen；It is described
The hydrofluoric acid for being 10% comprising volume fraction in mixed solution, 10% ethyl alcohol, remaining is deionized water；
B, start annealing furnace, and be filled with protective gas, temperature is risen to 760 DEG C, 25 minutes is kept the temperature, is put into monocrystalline silicon piece,
Again at 760 DEG C, 10 minutes are kept the temperature；
C, the temperature of annealing furnace is down to 660 DEG C, keeps the temperature 10 minutes；
D, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is put into Feng Lin mechanism, a Lateral supply a, side air-out is sent
Air port is equipped with condensation unit and cools down to air inlet, and cold air is blowed to monocrystalline silicon piece, wind speed 7m/s, air themperature 10 by blower
DEG C, monocrystalline silicon piece is placed on intermediate air duct, and cold wind is allowed to blow over lower planes from side, guarantees that two sides are uniform,
In 5min, monocrystalline silicon piece is cooled to room temperature；Temperature lowering curve function are as follows:T
It is the time s of cooling for rate of temperature fall DEG C/s, t, v is wind speed m/s, and C is specific heat capacity=0.219cal/gk of monocrystalline silicon, and R is
The radius cm, H of monocrystalline silicon are that the thickness cm, ρ of silicon wafer are the density 2.33g/cm of monocrystalline silicon3。
Embodiment 4
A, monocrystalline silicon is put into the mixed solution of hydrofluoric acid, ethyl alcohol and deionized water and is cleaned, then with being dried with nitrogen；It is described
The hydrofluoric acid for being 9% comprising volume fraction in mixed solution, 16% ethyl alcohol, remaining is deionized water；
B, start annealing furnace, and be filled with protective gas, temperature is risen to 743 DEG C, 25~35 minutes is kept the temperature, is put into monocrystalline silicon
Piece keeps the temperature 35 minutes again at 745 DEG C；
C, the temperature of annealing furnace is down to 644 DEG C, keeps the temperature 15 minutes；
D, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is put into Feng Lin mechanism, a Lateral supply a, side air-out is sent
Air port is equipped with condensation unit and cools down to air inlet, and cold air is blowed to monocrystalline silicon piece, wind speed 6m/s, air themperature 12 by blower
DEG C, monocrystalline silicon piece is placed on intermediate air duct, and cold wind is allowed to blow over lower planes from side, guarantees that two sides are uniform,
In 4min, monocrystalline silicon piece is cooled to room temperature；Temperature lowering curve function are as follows:T
It is the time s of cooling for rate of temperature fall DEG C/s, t, v is wind speed m/s, and C is specific heat capacity=0.219cal/gk of monocrystalline silicon, and R is
The radius cm, H of monocrystalline silicon are that the thickness cm, ρ of silicon wafer are the density 2.33g/cm of monocrystalline silicon3。
Embodiment 5
A, monocrystalline silicon is put into the mixed solution of hydrofluoric acid, ethyl alcohol and deionized water and is cleaned, then with being dried with nitrogen；It is described
The hydrofluoric acid for being 9% comprising volume fraction in mixed solution, 13% ethyl alcohol, remaining is deionized water；
B, start annealing furnace, and be filled with protective gas, temperature is risen to 755 DEG C, 32 minutes is kept the temperature, is put into monocrystalline silicon piece,
Again at 755 DEG C, 32 minutes are kept the temperature；
C, the temperature of annealing furnace is down to 655 DEG C, keeps the temperature 35 minutes；
D, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is put into Feng Lin mechanism, a Lateral supply a, side air-out is sent
Air port is equipped with condensation unit and cools down to air inlet, and cold air is blowed to monocrystalline silicon piece, wind speed 5m/s, air themperature 11 by blower
DEG C, monocrystalline silicon piece is placed on intermediate air duct, and cold wind is allowed to blow over lower planes from side, guarantees that two sides are uniform,
In 4min, monocrystalline silicon piece is cooled to room temperature；Temperature lowering curve function are as follows:T
It is the time s of cooling for rate of temperature fall DEG C/s, t, v is wind speed m/s, and C is specific heat capacity=0.219cal/gk of monocrystalline silicon, and R is
The radius cm, H of monocrystalline silicon are that the thickness cm, ρ of silicon wafer are the density 2.33g/cm of monocrystalline silicon3。
Comparative example 1
A, monocrystalline silicon is put into the mixed solution of hydrofluoric acid, ethyl alcohol and deionized water and is cleaned, then with being dried with nitrogen；It is described
The hydrofluoric acid for being 8% comprising volume fraction in mixed solution, 15% ethyl alcohol, remaining is deionized water；
B, start annealing furnace, and be filled with protective gas, temperature is risen to 750 DEG C, 30 minutes is kept the temperature, is put into monocrystalline silicon piece,
Again at 750 DEG C, 30 minutes are kept the temperature；
C, the temperature of annealing furnace is down to 650 DEG C, keeps the temperature 30 minutes；
D, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is cooled to room temperature in a natural environment.
Comparative example 2
A, monocrystalline silicon is put into the mixed solution of hydrofluoric acid, ethyl alcohol and deionized water and is cleaned, then with being dried with nitrogen；It is described
The hydrofluoric acid for being 8% comprising volume fraction in mixed solution, 15% ethyl alcohol, remaining is deionized water；
B, start annealing furnace, and be filled with protective gas, temperature is risen to 750 DEG C, 30 minutes is kept the temperature, is put into monocrystalline silicon piece,
Again at 750 DEG C, 30 minutes are kept the temperature；
C, the temperature of annealing furnace is down to 650 DEG C, keeps the temperature 30 minutes；
D, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is put into Feng Lin mechanism, a Lateral supply a, side air-out is sent
Air port is equipped with condensation unit and cools down to air inlet, and cold air is blowed to monocrystalline silicon piece by blower, and monocrystalline silicon piece is placed on centre
On air duct, and cold wind is allowed to blow over lower planes from side, guarantees that two sides are uniform, with cool down per minute 3 degree rate of temperature fall it is even
Speed cools down.
Comparative example 3
A, monocrystalline silicon is put into the mixed solution of hydrofluoric acid, ethyl alcohol and deionized water and is cleaned, then with being dried with nitrogen；It is described
The hydrofluoric acid for being 8% comprising volume fraction in mixed solution, 15% ethyl alcohol, remaining is deionized water；
B, start annealing furnace, and be filled with protective gas, temperature is risen to 750 DEG C, 30 minutes is kept the temperature, is put into monocrystalline silicon piece,
Again at 750 DEG C, 30 minutes are kept the temperature；
C, the temperature of annealing furnace is down to 650 DEG C, keeps the temperature 30 minutes；
D, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is put into Feng Lin mechanism, a Lateral supply a, side air-out is sent
Air port is equipped with condensation unit and cools down to air inlet, and cold air is blowed to monocrystalline silicon piece by blower, and monocrystalline silicon piece is placed on centre
On air duct, and cold wind is allowed to blow over lower planes from side, guarantees that two sides are uniform, temperature lowering curve function are as follows:
Data analysis
Respectively to the monocrystalline silicon piece via embodiment 1-5, comparative example 1-3 treated monocrystalline silicon piece and unannealed processing
Carry out resistivity measurement；Test result is shown in Table 1
Resistivity testing table 1 (unit: ohm)
| Test point 1 | Test point 2 | Test point 3 | Test point 4 | Test point 5 | Test point 6 | Test point 7 | Test point 8 | Test point 9 | |
| Embodiment 1 | 78.36 | 79.15 | 88.39 | 88.97 | 87.20 | 78.94 | 98.15 | 88.51 | 80.88 |
| Embodiment 2 | 81.68 | 85.43 | 90.46 | 91.23 | 93.24 | 81.38 | 102.73 | 92.67 | 81.09 |
| Embodiment 3 | 79.52 | 89.64 | 89.99 | 92.47 | 92.98 | 82.97 | 101.97 | 91.49 | 81.83 |
| Embodiment 4 | 79.13 | 81.34 | 89.01 | 89.07 | 89.64 | 79.83 | 99.53 | 89.67 | 80.67 |
| Embodiment 5 | 78.52 | 80.99 | 90.32 | 90.78 | 91.68 | 79.63 | 99.78 | 89.54 | 80.76 |
| Comparative example 1 | 108.94 | 118.43 | 99.44 | 117.46 | 105.68 | 95.99 | 109.22 | 96.76 | 92.68 |
| Comparative example 2 | 90.56 | 106.45 | 94.90 | 107.53 | 99.78 | 93.65 | 104.53 | 93.42 | 89.55 |
| Comparative example 3 | 87.45 | 90.64 | 96.53 | 103.27 | 98.26 | 89.66 | 103.23 | 92.67 | 86.74 |
| It is unannealed | 117.54 | 118.73 | 132.58 | 135.26 | 118.41 | 118.41 | 128.96 | 105.34 | 95.33 |
Test point 1 is the center of monocrystalline silicone disc, and test point 2-9 is uniformly arranged in the periphery of test point 1, and with it is described
60 centimetres of 1 distance of test point, as can be seen from table 1, the resistivity of the monocrystalline silicon piece by annealing is substantially better than unannealed
's；And use the method for the present invention temperature lowering curve resistivity be less than other method for annealing, and have resistance stabilization, float compared with
Small advantage.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and shown here as.
Claims (6)
1. a kind of method for annealing of monocrystalline silicon piece, includes:
A, start annealing furnace, and be filled with protective gas, temperature is risen to 740~760 DEG C, 25~35 minutes is kept the temperature, is put into monocrystalline
Silicon wafer keeps the temperature 10~40 minutes again at 740~760 DEG C；
B, the temperature of annealing furnace is down to 640~660 DEG C, keeps the temperature 10~40 minutes；
C, monocrystalline silicon piece is removed rapidly outside the annealing furnace, is put into Feng Lin mechanism, a Lateral supply, a side air-out, air outlet
Cool down equipped with condensation unit to air inlet, cold air is blowed into monocrystalline silicon piece by blower, wind speed is 3~7m/s, air themperature 10
~16 DEG C, monocrystalline silicon piece is placed on intermediate air duct, and cold wind is allowed to blow over lower planes from side, guarantees that two sides are equal
It is even, in 3~5min, monocrystalline silicon piece is cooled to room temperature；
Wherein, in step c, temperature lowering curve function are as follows:
T is rate of temperature fall DEG C/s, and t is the time s of cooling, and v is wind speed m/s, and C is the specific heat capacity C=0.219cal/ of monocrystalline silicon
Gk, R are the density 2.33g/cm of monocrystalline silicon for the thickness cm, ρ that the radius cm, H of monocrystalline silicon are silicon wafer3。
2. the method for annealing of monocrystalline silicon piece according to claim 1, it is characterised in that: the protective gas described in step a
For argon gas.
3. the method for annealing of monocrystalline silicon piece according to claim 1, it is characterised in that: be put into monocrystalline silicon piece in step a
Afterwards at 750 DEG C, keep the temperature 30 minutes.
4. the method for annealing of monocrystalline silicon piece according to claim 1, it is characterised in that: in stepb, by the temperature of annealing furnace
Degree is down to 650 DEG C, keeps the temperature 30 minutes.
5. the method for annealing of monocrystalline silicon piece according to claim 1, it is characterised in that: in step c, wind speed 4m/s,
Air themperature is 14 DEG C.
6. the method for annealing of monocrystalline silicon piece according to claim 1, it is characterised in that: cope with the monocrystalline before step a
Silicon wafer is pre-processed, and the pretreated method is the mixed solution that monocrystalline silicon is put into hydrofluoric acid, ethyl alcohol and deionized water
Middle cleaning, then with being dried with nitrogen；The hydrofluoric acid for being 5~10% comprising volume fraction in the mixed solution, 10~20% second
Alcohol, remaining is deionized water.
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| CN115369486A (en) * | 2022-10-26 | 2022-11-22 | 新美光(苏州)半导体科技有限公司 | Method for solving problem of false height of resistance and inversion of conductivity type of abnormal silicon rod |
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| CN115369486A (en) * | 2022-10-26 | 2022-11-22 | 新美光(苏州)半导体科技有限公司 | Method for solving problem of false height of resistance and inversion of conductivity type of abnormal silicon rod |
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