CN114921846A - Method for reducing impurity stripe of heavy antimony doped 100 monocrystal - Google Patents
Method for reducing impurity stripe of heavy antimony doped 100 monocrystal Download PDFInfo
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- CN114921846A CN114921846A CN202210604027.6A CN202210604027A CN114921846A CN 114921846 A CN114921846 A CN 114921846A CN 202210604027 A CN202210604027 A CN 202210604027A CN 114921846 A CN114921846 A CN 114921846A
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- 239000012535 impurity Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 18
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000013078 crystal Substances 0.000 claims abstract description 154
- 238000007711 solidification Methods 0.000 claims abstract description 13
- 230000008023 solidification Effects 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 36
- 229910052786 argon Inorganic materials 0.000 claims description 18
- 230000005484 gravity Effects 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 2
- 230000007423 decrease Effects 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052710 silicon Inorganic materials 0.000 abstract description 16
- 239000010703 silicon Substances 0.000 abstract description 16
- 239000013256 coordination polymer Substances 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 description 34
- 235000012431 wafers Nutrition 0.000 description 19
- 230000004075 alteration Effects 0.000 description 10
- 238000004321 preservation Methods 0.000 description 10
- 201000010099 disease Diseases 0.000 description 8
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 8
- 210000003128 head Anatomy 0.000 description 7
- 238000010621 bar drawing Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 235000014347 soups Nutrition 0.000 description 2
- 244000208734 Pisonia aculeata Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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
- 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
-
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a method for reducing the stripe of antimony heavily doped <100> single crystal impurities, which belongs to the technical field of silicon Wafer processing, and the method controls the growth interface of a crystal bar by controlling the pulling speed of the crystal bar when the crystal bar is pulled, controls the growth interface of a concave solution to be horizontal or convex so as to ensure that the solidification time of the growth interface of the crystal bar is the same, further ensures that the radial solidification time is the same in the cutting direction vertical to the growth axis direction, ensures that the concentration of the impurities at each point is consistent, further does not generate concentric circles or eccentric circular stripes on the Wafer surface after CP corrosion, and ensures that the yield of products is not reduced.
Description
Technical Field
The invention relates to the technical field of silicon wafer processing, in particular to a method for reducing stripes of heavily antimony doped (100) single crystal impurities.
Background
After the crystal bar is drawn, the crystal bar is cut into silicon wafers, impurity stripes appear on the surfaces of the silicon wafers, the impurity stripes are represented as regular concentric circular stripes or eccentric circular stripes or irregular stripes (the regularity refers to chromatic aberration stripes visible on the surfaces of the silicon wafers), if the impurity stripes appear as irregular stripes, the impurity stripes are generally oxygen stripes, and if the impurity stripes appear as regular concentric circular stripes or eccentric circular stripes, the impurity stripes generally appear as resistivity stripes.
In the prior art, concentric circles or eccentric circular patterns appear on the surface of a Wafer (Wafer) subjected to mixed acid Corrosion (CP) of a crystal bar with antimony heavily doped in the crystal orientation, impurity concentration shows a high head-to-tail trend due to a segregation effect of doping, and resistivity shows a high head-to-tail trend, so that the tail resistivity of the crystal bar is low, the probability of the concentric circles or the eccentric circular patterns appearing at the tail of the crystal bar is high, and when the crystal bar is cut into a silicon Wafer, a part of the silicon Wafer is subjected to ring pattern color difference observation by naked eyes to exceed a limit sample (the limit sample shows that unclear stripes exist on the surface of the silicon Wafer and are difficult to observe by the naked eyes), so that the silicon Wafer is scrapped and the yield is influenced.
Disclosure of Invention
In view of the above, the present invention provides a method for reducing stripes of antimony heavily doped <100> single crystal impurities, so as to solve the technical problem that in the prior art, after a <100> crystal orientation antimony heavily doped crystal bar is cut into silicon wafers, part of the silicon wafers exceed a limit sample through naked eye observation of ring grain color difference, so that the silicon wafers are scrapped, and the yield is affected.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for reducing the stripe of the impurity of a heavily antimony doped <100> single crystal controls the growth interface of a crystal bar by controlling the pulling speed of the crystal bar when the crystal bar is pulled, and controls the growth interface concave to a solution into a horizontal shape or a convex shape so as to ensure that the solidification time of the growth interface of the crystal bar is the same.
Preferably, after 70% of the crystal bar is drawn, drawing the crystal bar at a drawing speed of 0-0.6mm/min, gradually reducing the drawing speed along with the drawing of the crystal bar, and controlling the average drawing speed to be-10% so as to control the growth interface of the concave solution to be horizontal or convex.
Preferably, before the crystal bar is drawn, the upper and lower limit drawing speeds of the crystal bar are set to be-0.25 mm/min.
Preferably, the ratio of the crystal bar rotating speed to the crucible rotating speed is controlled to be more than 1 when the crystal bar is pulled, namely: SR/CR >1.0 to stabilize the solid-liquid interface.
Preferably, argon gas is introduced at a predetermined flow rate while the ingot is being pulled.
Preferably, the predetermined flow rate of argon is 0 to 80 slm.
Preferably, before opening the furnace, the deviation of the center shaft axis in the single crystal furnace from the cross direction of the furnace barrel, the heat preservation barrel and the heater is ensured to be less than a first preset distance, and the deviation of the center shaft axis from the gravity center of the heavy hammer is ensured to be less than a second preset distance.
Preferably, the first predetermined distance is 3 mm.
Preferably, the second predetermined distance is 3 mm.
Preferably, the diameter of the crystal bar is controlled only by adjusting the temperature when the change of the diameter of the crystal bar is large in the process of drawing the crystal bar.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, when the crystal bar is drawn, the growth interface concave to the melt is controlled to be horizontal or convex by controlling the growth interface of the crystal bar, so that the solidification time of the growth interface of the crystal bar is the same, and further the radial solidification time is the same in the cutting direction vertical to the growth axis direction, so that the concentrations of impurities at each point are consistent, and further no concentric circle or eccentric circular ring pattern appears on the Wafer surface after CP corrosion, so that the yield of products is not reduced.
Detailed Description
The technical solution and the technical effects of the present invention are further described in detail below.
A method for reducing the stripe of the impurity of a heavily antimony doped <100> single crystal controls the growth interface of a crystal bar by controlling the pulling speed of the crystal bar when the crystal bar is pulled, and controls the growth interface concave to a solution into a horizontal shape or a convex shape so as to ensure that the solidification time of the growth interface of the crystal bar is the same.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, when the crystal bar is drawn, the growth interface of the concave solution is controlled to be horizontal or convex by controlling the growth interface of the crystal bar, so that the solidification time of the growth interface of the crystal bar is the same, and further the radial solidification time is the same in the cutting direction vertical to the growth axis direction, so that the concentration of impurities at each point is consistent, and further concentric circles or eccentric circular patterns cannot appear on the Wafer surface after CP corrosion, so that the yield of products cannot be reduced.
Further, after 70% of the crystal bar is drawn, drawing the crystal bar at a drawing speed of 0-0.6mm/min, gradually reducing the drawing speed along with the drawing of the crystal bar, and controlling the average drawing speed to be-10% so as to control the growth interface of the concave solution to be horizontal or convex.
Specifically, the average pulling rate is an average value in unit time, the unit time is set to 2h, and the calculation method of the fluctuation value is as follows: (average pull-up rate-set pull-up rate)/set pull-up rate 100%, the pull-up rate fluctuation of the constant diameter head may not be counted in.
Furthermore, before the crystal bar is drawn, the upper limit drawing speed and the lower limit drawing speed of the crystal bar are set to be-0.25 mm/min, so that the drawing speed does not change too much in the changing process, and the diameter of the crystal bar is not influenced.
Further, when the crystal bar is pulled, the ratio of the crystal bar rotating speed to the crucible rotating speed is controlled to be larger than 1, namely: SR/CR >1.0, the direction that the crystal bar rotates is different with the direction that the crucible rotated, and the crystal bar rotates and rotates the different forced convection that brings two kinds of directions with the crucible, and wherein the forced convection that the crystal bar rotated and arouses can restrain natural convection, increases the crystal and changes the solid-liquid interface (CZ) that the crucible energy ratio can be better stable, radial impurity distribution of effectual control for radial impurity distribution is even.
Further, when the crystal bar is drawn, argon gas with preset flow is introduced
Further, the preset flow rate of the argon is 0-80slm, and the preset flow rate of the argon and the Gap value are introduced to stabilize the surface of the molten soup.
In particular, because of the heavy doping of antimony (6 in)ch) is distributed between 0.01 and 0.02 omega cm, and the concentration of antimony in the silicon is 3.6E18-9.4E18atom/cm 3 In the method, the represented impurity stripes are resistivity stripes and concentric circle or eccentric circle annular stripes, because of the segregation effect of doping, the resistivity can show the trend of high head and low tail, the impurity concentration shows the trend of low head and high tail, so that the probability of the impurity stripes appearing at the tail of the crystal bar is higher, in the prior art, the probability of the annular stripes is easily reduced by improving the resistivity due to the fact that the resistivity can show the trend of high head and low tail, but the invention sets a lower pulling speed after the crystal bar is drawn by 70 percent by setting process parameters, controls the growth interface of a concave solution to be horizontal or convex, controls the average pulling speed fluctuation to be within-10 percent, controls the crystal rotation and crucible rotation ratio, sets a proper argon flow and a Gap value, stabilizes the surface of molten soup, stabilizes a solid-liquid interface, and the solidification time of the growth interface of the crystal bar is the same, and then in the cutting direction vertical to the growth axis direction, the radial solidification time is the same, so that the concentration of impurities at each point is consistent, concentric circles or eccentric circular ring patterns cannot appear on the Wafer surface after CP corrosion, and the yield of products cannot be reduced.
Furthermore, before opening the furnace, the deviation of the center shaft axis in the single crystal furnace with the cross direction of the furnace barrel, the heat preservation barrel and the heater is smaller than a first preset distance, and the deviation of the center shaft axis and the gravity center of the heavy hammer is confirmed to be smaller than a second preset distance, so that the center of a circle of a growth interface is consistent with the center shaft axis in the single crystal furnace, and further, the occurrence of eccentric annular grains is avoided.
Specifically, the precision of the single crystal furnace is as follows: 0.05 rpm; CR: 0.05 rpm; seed crystal lifting Speed (SL): plus or minus 0.05 mm/min; crucible lifting speed (CL): 0.01 mm/min; flow rate of argon (Ar): 1 slm; liquid Gap (Gap): plus or minus 2 mm.
Further, the first predetermined distance is 3 mm.
Further, the second predetermined distance is 3 mm.
Furthermore, in the crystal bar drawing process, if the diameter of the crystal bar changes greatly, the diameter of the crystal bar is controlled only by adjusting the temperature, but not by adjusting the drawing speed, and the shape of a crystal bar growth interface is influenced by adjusting the drawing speed.
Further, the resistivity is improved in the resistivity specification, so that the position of the ring grain is close to the tail of the crystal bar; because the existing resistivity specification and the segregation coefficient of antimony (K = 0.023) cannot eliminate the ring grain by increasing the resistivity, the resistivity can be increased only in the resistivity specification to ensure that the ring grain is generated at a position close to the tail part of the crystal bar, so that the ring grain defect rate can be reduced by solving the problem of the ring grain occurrence rate and serious conditions of the tail part.
Specifically, the occurrence position of the ring grain is changed by increasing the resistivity within the resistivity specification, and the specific experimental process is detailed in experiment 1.
Experiment 1: the precision of the single crystal furnace is SR: 0.05 rpm; CR: 0.05 rpm; SL: 0.05 mm/min; CL: 0.01 mm/min; ar: 1 slm; and (4) Gap: +/-2 mm, detecting that the cross direction of the center axis in the single crystal furnace and the furnace cylinder, the heat preservation cylinder and the heater is less than 3mm, confirming that the deviation of the center axis and the gravity center of the heavy hammer is less than 3mm, SL =0.80mm/min after the length of the crystal bar is 70%, the fluctuation range of the pulling speed is-10-10%, the upper limit and the lower limit of the pulling speed are-0.25-0.25 mm/min, SR/CR =1.5, the flow of argon is 80slm, when the resistivity specification is 0.008-0.02 omega-cm, drawing the crystal bar, dividing the experiment into 3 groups according to the head resistivity, carrying out 5 times of experiments on each group, and obtaining data as shown in table 1 except the resistivity.
TABLE 1
| Group of | Serial number | Resistivity of head | The ratio of ring grain generation position to crystal bar | Severity of disease |
| A | 1 | 0.016 | 61% | Is not acceptable |
| A | 2 | 0.016 | 60% | Is not acceptable |
| A | 3 | 0.016 | 59% | Is not acceptable |
| A | 4 | 0.016 | 64% | Is not acceptable |
| A | 5 | 0.016 | 63% | Is not acceptable |
| B | 1 | 0.0175 | 65% | Is not acceptable |
| B | 2 | 0.0175 | 67% | Is not acceptable |
| B | 3 | 0.0175 | 69% | Is not acceptable |
| B | 4 | 0.0175 | 65% | Is not acceptable |
| B | 5 | 0.0175 | 66% | Is not acceptable |
| C | 1 | 0.0185 | 70% | Is not acceptable |
| C | 2 | 0.0185 | 71% | Is not acceptable |
| C | 3 | 0.0185 | 74% | Is not acceptable |
| C | 4 | 0.0185 | 72% | Is not acceptable |
| C | 5 | 0.0185 | 72% | Is not acceptable |
Through table 1 experimental data, it can be seen that concentric circular ring lines still can appear on the surface of a silicon wafer with increased resistivity, the chromatic aberration of the ring lines is higher than that of a limit sample, scrapping can be caused, the yield is affected, the position where the ring lines occur can be closer to the tail of a crystal bar due to increased resistivity, the utilization rate of the crystal bar is improved, and scrapped parts are reduced.
Specifically, the process of the invention is determined, and the specific experimental process is shown in experiment 2-experiment 6.
Experiment 2: the precision of the single crystal furnace is SR: 0.05 rpm; CR: 0.05 rpm; SL: 0.05 mm/min; CL: plus or minus 0.01 mm/min; ar: 1 slm; and (4) Gap: +/-2 mm, detecting that the cross direction of the center shaft axis in the single crystal furnace and the furnace barrel, the heat preservation barrel and the heater is less than 3mm, confirming that the deviation between the center shaft axis and the gravity center of the heavy hammer is less than 3mm, carrying out experiments under TOP Res =0.0185, carrying out crystal bar drawing, dividing the experiments into 5 groups according to the set value of 70% later pulling speed of the crystal bar, carrying out 5 times of experiments on each group, and obtaining data shown in table 2 except the resistivity with the same parameters.
TABLE 2
| Group of | Serial number | 70% pull-back speed setting | The ratio of ring grain generation position to crystal bar | Severity of disease |
| A | 1 | 0.80mm/min | 60% | Is not acceptable |
| A | 2 | 0.80mm/min | 61% | Is not acceptable |
| A | 3 | 0.80mm/min | 59% | Is not acceptable |
| A | 4 | 0.80mm/min | 58% | Is not acceptable |
| A | 5 | 0.80mm/min | 62% | Is not acceptable |
| B | 1 | 0.70mm/min | 67% | Is not acceptable |
| B | 2 | 0.70mm/min | 69% | Is not acceptable |
| B | 3 | 0.70mm/min | 70% | Is not acceptable |
| B | 4 | 0.70mm/min | 71% | Is not acceptable |
| B | 5 | 0.70mm/min | 69% | Is not acceptable |
| C | 1 | 0.60mm/min | 78% | Can accept |
| C | 2 | 0.60mm/min | 79% | Can accept |
| C | 3 | 0.60mm/min | 79% | Can accept |
| C | 4 | 0.60mm/min | 80% | Can accept |
| C | 5 | 0.60mm/min | 81% | Can accept |
| D | 1 | 0.55mm/min | 82% | Can accept |
| D | 2 | 0.55mm/min | 83% | Can accept |
| D | 3 | 0.55mm/min | 80% | Can accept |
| D | 4 | 0.55mm/min | 79% | Can accept |
| D | 5 | 0.55mm/min | 81% | Can accept |
| E | 1 | 0.52mm/min | 82% | Can accept it |
| E | 2 | 0.52mm/min | 83% | Can accept |
| E | 3 | 0.52mm/min | 84% | Can accept |
| E | 4 | 0.52mm/min | 82% | Can accept |
| E | 5 | 0.52mm/min | 81% | Can accept |
| F | 1 | 0.50mm/min | 84% | Can accept |
| F | 2 | 0.50mm/min | 85% | Can accept |
| F | 3 | 0.50mm/min | 85% | Can accept |
| F | 4 | 0.50mm/min | 84% | Can accept it |
| F | 5 | 0.50mm/min | 83% | Can accept it |
As can be seen from Table 2, when the pulling rate of the ingot after 70% of the length of the ingot is set to 0.7mm/min to 0.8mm/min, the chromatic aberration of the ring grains of the entire ingot is higher than that of the limit sample, which may result in rejection and affect the yield, but when the pulling rate of the ingot after 70% of the length of the ingot is set to 0.6mm/min to 0.5mm/min, the growth interface of the entire ingot during growth is horizontal or convex, which may result in the chromatic aberration of the ring grains of the entire ingot being lower than that of the limit sample, which may result in the availability and no rejection of the entire ingot, but when the pulling rate of the ingot after 70% of the length of the ingot is set to 0.50mm/min, which may result in crystal pulling failure, the optimal pulling rate of the ingot after 70% of the length of the ingot is set to 0.6mm/min to 0.52 mm/min.
Experiment 3: the precision of the single crystal furnace is as follows: 0.05 rpm; CR: 0.05 rpm; SL: 0.05 mm/min; CL: 0.01 mm/min; ar: 1 slm; and (4) a Gap: +/-2 mm, detecting that the cross direction of the central axis in the single crystal furnace and the furnace cylinder, the heat preservation cylinder and the heater is less than 3mm, confirming that the deviation of the central axis and the gravity center of the heavy hammer is less than 3mm, performing an experiment with SL =0.60mm/min after TOP Res =0.0185 and the length of the crystal bar is 70%, drawing the crystal bar to ensure that the growth interface of the whole crystal bar is horizontal or convex during growth, dividing the experiment into 2 groups according to the fluctuation range of the drawing speed, performing 5 times of experiments on each group, and obtaining the data as shown in Table 3, wherein other parameters are the same.
TABLE 3
| Group of | Serial number | Range of fluctuation | The ratio of ring grain generation position to crystal bar | Severity of disease |
| A | 1 | ±10% | 78% | Can accept |
| A | 2 | ±10% | 79% | Can accept it |
| A | 3 | ±10% | 80% | Can accept it |
| A | 4 | ±10% | 79% | Can accept it |
| A | 5 | ±10% | 81% | Can accept |
| B | 1 | ±5% | 84% | Can accept it |
| B | 2 | ±5% | 83% | Can accept |
| B | 3 | ±5% | 84% | Can accept it |
| B | 4 | ±5% | 83% | Can accept |
| B | 5 | ±5% | 82% | Can accept |
It can be seen from table 3 that the pulling rate fluctuation range is in the range of-10% to 10%, the chromatic aberration of the ring grains of the entire crystal bar is lower than the limit sample, so that the entire crystal bar can be used and cannot be discarded, when the pulling rate fluctuation range is larger, although the chromatic aberration of the ring grains is lower than the limit sample, the quality of the crystal bar is affected by the ratio of the ring grain generation position to the crystal bar closer to the head of the crystal bar, when the pulling rate fluctuation range is smaller, the ring grain generation position is closer to the tail of the crystal bar, the use range of the crystal bar is wider and the use frequency is higher, and because the precision of the equipment is limited, an experiment with smaller pulling rate fluctuation is not performed, but according to the experiment, the ring grain generation position occupies the tail of the crystal bar closer to the smaller pulling rate fluctuation.
Experiment 4: the precision of the single crystal furnace is as follows: 0.05 rpm; CR: 0.05 rpm; SL: 0.05 mm/min; CL: plus or minus 0.01 mm/min; ar: plus or minus 1 slm; and (4) Gap: +/-2 mm, detecting that the cross direction of the center axis in the single crystal furnace and the furnace barrel, the heat preservation barrel and the heater is less than 3mm, confirming that the center axis deviation and the gravity center deviation of the heavy hammer are less than 3mm, carrying out experiments under the conditions that TOP Res =0.0185, SL =0.60mm/min after the crystal bar is 70% in length and the pulling speed fluctuation range is-5-5%, drawing the crystal bar to ensure that the growth interface of the whole crystal bar is horizontal or convex during growth, dividing the experiments into 2 groups according to the setting of the upper limit and the lower limit of the pulling speed, carrying out 5 experiments on each group, and obtaining the same parameters as shown in Table 4.
TABLE 4
| Group of | Serial number | Upper and lower limit of pulling speed/mm/min | The ratio of ring grain generation position to crystal bar | Severity of disease |
| A | 1 | -0.25-0.25 | 84% | Can accept it |
| A | 2 | -0.25-0.25 | 83% | Can accept |
| A | 3 | -0.25-0.25 | 84% | Can accept |
| A | 4 | -0.25-0.25 | 82% | Can accept it |
| A | 5 | -0.25-0.25 | 84% | Can accept |
| B | 1 | -0.2-0.2 | 85% | Can accept it |
| B | 2 | -0.2-0.2 | 85% | Can accept |
| B | 3 | -0.2-0.2 | 86% | Can accept it |
| B | 4 | -0.2-0.2 | 85% | Can accept it |
| B | 5 | -0.2-0.2 | 84% | Can accept it |
As can be seen from Table 4, the upper and lower limits of the pulling rate are set at-0.25-0.25 mm/min, and the chromatic aberration of the ring grains of the whole crystal bar is lower than the limit sample, so that the whole crystal bar can be used without being scrapped.
Experiment 5: the precision of the single crystal furnace is as follows: 0.05 rpm; CR: 0.05 rpm; SL: 0.05 mm/min; CL: plus or minus 0.01 mm/min; ar: 1 slm; and (4) Gap: +/-2 mm, detecting that the cross direction of the central axis in the single crystal furnace and the furnace cylinder, the heat preservation cylinder and the heater is less than 3mm, confirming that the deviation of the central axis and the gravity center of the heavy hammer is less than 3mm, carrying out experiments under the conditions that TOP Res =0.0185, SL =0.60mm/min after the length of the crystal bar is 70%, the fluctuation range of the pulling speed is-5-5%, and the upper limit and the lower limit of the pulling speed are-0.2-0.2 mm/min, carrying out crystal bar drawing, enabling the growth interface of the whole crystal bar to be horizontal or convex during growth, dividing the experiments into 3 groups according to the difference of SR/CR, carrying out 5 times of experiments on each group, and obtaining data as shown in table 5, wherein other parameters are the same.
TABLE 5
| Group of | Serial number | SR/CR | The ratio of ring grain generation position to crystal bar | Severity of disease |
| A | 1 | 1.5 | 85% | Can accept |
| A | 2 | 1.5 | 85% | Can accept |
| A | 3 | 1.5 | 85% | Can accept |
| A | 4 | 1.5 | 84% | Can accept it |
| A | 5 | 1.5 | 84% | Can accept |
| B | 1 | 1.7 | 86% | Can accept |
| B | 2 | 1.7 | 85% | Can accept |
| B | 3 | 1.7 | 86% | Can accept |
| B | 4 | 1.7 | 85% | Can accept |
| B | 5 | 1.7 | 86% | Can accept |
| C | 1 | 2.0 | 87% | Can accept |
| C | 2 | 2.0 | 86% | Can accept |
| C | 3 | 2.0 | 88% | Can accept it |
| C | 4 | 2.0 | 88% | Can accept |
| C | 5 | 2.0 | 87% | Can accept it |
As can be seen from table 5, when the SR/CR is greater than 1, the chromatic aberration of the ring grain generated on the entire crystal bar is lower than the limit sample, so that the entire crystal bar is usable and cannot be scrapped, and the higher the SR/CR value is, the closer the ring grain generation position is to the tail of the crystal bar, the higher the yield of the crystal bar is, and because the precision of the equipment is limited, no experiment with larger SR/CR is performed, but according to the above experiment, the larger the SR/CR is, the larger the ring grain generation position occupies the closer to the tail of the crystal bar, and the higher the quality of the silicon wafer is; and the resonance point is avoided when setting the specific crystal rotation value and pot rotation value according to the SR/CR ratio.
Experiment 6: the precision of the single crystal furnace is SR: 0.05 rpm; CR: 0.05 rpm; SL: plus or minus 0.05 mm/min; CL: plus or minus 0.01 mm/min; ar: 1 slm; and (4) Gap: +/-2 mm, detecting that the cross direction of the central axis in the single crystal furnace and the furnace barrel, the heat preservation barrel and the heater is less than 3mm, confirming that the deviation of the central axis and the gravity center of the heavy hammer is less than 3mm, carrying out experiments under TOP Res =0.0185 and SL =0.60mm/min after the length of the crystal bar is 70%, wherein the fluctuation range of the pulling speed is-5-5%, the upper limit and the lower limit of the pulling speed are-0.2-0.2 mm/min, and SR/CR =2.0, carrying out crystal bar drawing, so that the growth interface of the whole crystal bar is horizontal or convex during growth, dividing the experiments into 3 groups according to the difference of argon flow, carrying out 5 times of experiments on each group, and obtaining the data which are shown in table 6.
TABLE 6
| Group of | Serial number | Argon flow/slm | The ratio of ring grain generation position to crystal bar | Severity of disease |
| A | 1 | 40 | 85% | Can accept |
| A | 2 | 40 | 86% | Can accept |
| A | 3 | 40 | 85% | Can accept it |
| A | 4 | 40 | 85% | Can accept |
| A | 5 | 40 | 86% | Can accept it |
| B | 1 | 60 | 88% | Can accept |
| B | 2 | 60 | 89% | Can accept it |
| B | 3 | 60 | 89% | Can accept |
| B | 4 | 60 | 90% | Can accept |
| B | 5 | 60 | 88% | Can accept |
| C | 1 | 80 | 85% | Can accept |
| C | 2 | 80 | 83% | Can accept |
| C | 3 | 80 | 84% | Can accept |
| C | 4 | 80 | 84% | Can accept |
| C | 5 | 80 | 85% | Can accept |
It can be seen from table 6 that, when the argon flow is 40-80slm, the argon flow and the Gap value make the molten liquid surface stable, the fluctuation is small, the impurity distribution of the solid-liquid interface of the crystal bar, the chromatic aberration of the ring grain generated by the whole crystal bar is lower than the limit sample, the whole crystal bar is usable and can not be scrapped, and when the argon flow is 60slm, the closer the ring grain generating position is to the tail of the crystal bar, the higher the yield of the crystal bar is.
In summary, the best growth conditions for the ingot can be found in experiments 2 to 6 as follows: the upper limit resistance resistivity, SL =0.60mm/min, the pulling rate fluctuation range is +/-5%, the upper and lower limits of the pulling rate are +/-0.2 mm, SR/CR =2.0, and the argon gas is 50-70slm in the resistivity specification.
Specifically, this scheme is further illustrated by the following example 1 and comparative example 1.
Example 1
The precision of the single crystal furnace is as follows: 0.05 rpm; CR: 0.05 rpm; SL: 0.05 mm/min; CL: 0.01 mm/min; ar: 1 slm; and (4) Gap: +/-2 mm, detecting that the cross direction of the center axis in the single crystal furnace and the furnace cylinder, the heat preservation cylinder and the heater is less than 3mm, confirming that the deviation of the center axis and the gravity center of the heavy hammer is less than 3mm, carrying out crystal bar drawing under TOP Res =0.0185, SL =0.60mm/min after 70% of the crystal bar length, the fluctuation range of the drawing speed is-5-5%, the upper limit and the lower limit of the drawing speed are-0.2-0.2 mm/min, SR/CR =2.0 and the argon flow rate is 60slm, and carrying out 10 experiments totally to obtain the data shown in Table 7, wherein the growth interface of the whole crystal bar is horizontal or convex during growth.
TABLE 7
| Serial number | The ratio of ring grain generation position to crystal bar | Severity of disease |
| 1 | 88% | Can accept |
| 2 | 87% | Can accept it |
| 3 | 85% | Can accept |
| 4 | 89% | Can accept it |
| 5 | 88% | Can accept it |
| 6 | 85% | Can accept it |
| 7 | 86% | Can accept it |
| 8 | 90% | Can accept it |
| 9 | 88% | Can accept |
| 10 | 89% | Can accept it |
Comparative example 1
The precision of the single crystal furnace is SR: 0.05 rpm; CR: 0.05 rpm; SL: 0.05 mm/min; CL: 0.01 mm/min; ar: plus or minus 1 slm; and (4) Gap: +/-2 mm, detecting that the cross direction of the center axis in the single crystal furnace and the furnace barrel, the heat preservation barrel and the heater is less than 3mm, confirming that the deviation of the center axis and the gravity center of the heavy hammer is less than 3mm, carrying out crystal bar drawing under conditions that TOP Res =0.0185, SL =0.80mm/min after 70% of the crystal bar length, the drawing speed fluctuation range is-10-10%, the upper and lower limits of the drawing speed are-0.25-0.25 mm/min, SR/CR =1.5 and the argon flow is 80slm, so that the growth interface of the whole crystal bar is concave during growth, and carrying out 10 experiments totally to obtain the data shown in Table 8.
TABLE 8
| Serial number | The ratio of ring grain generation position to crystal bar | Severity of disease |
| 1 | 72% | Is not acceptable |
| 2 | 71% | Is not acceptable |
| 3 | 70% | Is not acceptable |
| 4 | 73% | Is not acceptable |
| 5 | 72% | Is not acceptable |
| 6 | 69% | Is not acceptable |
| 7 | 71% | Is not acceptable |
| 8 | 70% | Is not acceptable |
| 9 | 68% | Is not acceptable |
| 10 | 73% | Is not acceptable |
Through the experiments of the embodiment 1 and the comparative example 1, the process is improved, so that the growth interface of the whole crystal bar, which is concave to the solution, is controlled to be horizontal or convex during growth, the solidification time of the growth interface of the crystal bar is the same, the radial solidification time is the same in the cutting direction vertical to the growth axis direction, the concentration of impurities at each point is consistent, the chromatic aberration of the ring grains on the surface of the silicon wafer is lower than that of a limit sample, and the whole crystal bar can be used and cannot be scrapped.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
Claims (10)
1. A method for reducing the impurity fringes of a heavily antimony doped <100> single crystal is characterized in that the growth interface of the crystal rod is controlled by controlling the pulling speed of the crystal rod when the crystal rod is pulled, and the growth interface concave to a solution is controlled to be horizontal or convex so as to ensure that the solidification time of the growth interface of the crystal rod is the same.
2. The method according to claim 1, wherein after 70% of the ingot is pulled, the ingot is pulled at a pulling rate of 0-0.6mm/min, the pulling rate gradually decreases with the pulling of the ingot, and the average pulling rate fluctuation is-10 to 10% so that the growth interface of the concave portion to the melt is controlled to be horizontal or convex.
3. The method according to claim 2, wherein the upper and lower pulling speeds of the ingot are set to-0.25 to 0.25mm/min before the ingot is pulled.
4. The method for reducing the striations of antimony <100> heavily doped single crystal impurities as claimed in claim 3, wherein the ratio of the rotation speed of the ingot to the rotation speed of the crucible is controlled to be greater than 1 during the ingot pulling process, namely: SR/CR >1.0 to stabilize the solid-liquid interface.
5. The method for reducing striations of antimony <100> heavily doped single crystal impurities as claimed in claim 4, wherein a predetermined flow rate of argon is introduced during the ingot pulling.
6. The method of reducing striations of heavily antimony doped <100> single crystal impurities as claimed in claim 5, wherein said predetermined flow rate of argon is 0-80 slm.
7. The method according to claim 6, wherein before opening the furnace, the deviation of the center axis of the central axis of the single crystal furnace from the cross direction of the furnace barrel, the heat-preserving barrel and the heater is less than a first predetermined distance, and the deviation of the center axis of the central axis from the gravity center of the weight is determined to be less than a second predetermined distance.
8. The method of reducing striations of heavily antimony doped <100> single crystal impurities as claimed in claim 7, wherein said first predetermined distance is 3 mm.
9. The method of reducing striations of heavily antimony doped <100> single crystal impurities as claimed in claim 8, wherein said second predetermined distance is 3 mm.
10. The method of claim 9, wherein the diameter of the ingot is controlled by adjusting the temperature only if there is a large variation in the diameter of the ingot during the ingot pulling process.
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