CN113758905A - Quality judgment method of ingot casting single crystal silicon block and ingot casting single crystal silicon block - Google Patents
Quality judgment method of ingot casting single crystal silicon block and ingot casting single crystal silicon block Download PDFInfo
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Abstract
The invention discloses a quality judgment method of ingot casting monocrystalline silicon blocks and the ingot casting monocrystalline silicon blocks, which comprises the following steps: (1) uniformly removing the head of the ingot casting monocrystalline silicon block by about 30-60 mm; (2) measuring a photoluminescence test picture of the head end face of the ingot casting monocrystalline silicon block by using a photoluminescence tester, and calculating to obtain a black silk area proportion value D of the photoluminescence test pictureS(ii) a (3) Measuring and calculating the end surface area S of the ingot casting monocrystalline silicon block; (4) establishing a black silk growth calculation model, and determining the ratio value D of the removal length L of the silicon briquette to the area of the black silk on the preset end surfaceLIs a relational expression L (D)L⍺), wherein ⍺ is the dislocation growth angle; (5) according to the preset area proportion value D of the black silk on the end surfaceLAnd the relation L (D)L⍺), calculating the value of the silicon block removal length L; (6)and removing the head of the ingot casting monocrystalline silicon block according to the value of the silicon block removal length L. According to the method, a brand-new removing mode of different black silk proportions at the head of the ingot casting monocrystalline silicon block is provided by combining photoluminescence testing with the growth characteristics of the ingot casting monocrystalline silicon ingot.
Description
Technical Field
The invention relates to the technical field of ingot casting single crystal silicon ingot preparation, in particular to a quality judgment method of an ingot casting single crystal silicon block and the ingot casting single crystal silicon block.
Background
The growth of the polycrystalline nucleation of the ingot casting is small crystal grain nucleation, the growth quality of different areas is close to that of vertical columnar crystals, and the impurities at the head part of the ingot casting are more due to the segregation effect, so the head part removing judgment method of the polycrystalline silicon block of the ingot casting mainly takes the judgment of minority carrier lifetime representing the amount of the impurities in the silicon block as the main point; on the other hand, the czochralski single crystal is generally a dislocation-free single crystal, and when impurities or dislocations are present, the czochralski single crystal is grown into polycrystal by breaking the wire, and the head defect is mainly a resistivity defect due to oxygen donors or a diameter defect due to pulling, and therefore the method for determining the head removal of the czochralski single crystal silicon ingot is mainly based on the determination of the resistivity defect and the diameter defect.
The ingot casting single crystal is a silicon crystal product which is rapidly developed in recent years, the performance of the ingot casting single crystal is between that of ingot casting polycrystal and that of straight pulling single crystal, the ingot casting single crystal can be suitable for the alkali wool making process of the single crystal, the efficiency is far higher than that of the ingot casting polycrystal, the single feeding amount is large, and the production cost is far lower than that of the straight pulling single crystal. However, because the raw material of the ingot-casting monocrystalline silicon block is low in grade (the impurity content in the raw material is higher) compared with the raw material of the czochralski single crystal, and the growth mode is different from that of the czochralski single crystal, some dislocations exist in the ingot-casting monocrystalline silicon block, the efficiency of a battery piece prepared subsequently from the ingot-casting monocrystalline silicon block is seriously influenced, and if the head part is removed according to the judgment mode of the minority carrier lifetime of the ingot-casting polycrystalline silicon block and the judgment mode of the resistivity of the czochralski single crystal, a large error exists. In addition, the existing dislocation detection mode mainly adopts chemical corrosion, physical polishing and microscope observation, can only detect the dislocation density of a local area of a single silicon wafer each time, is mainly used for research and development guidance, and cannot be used for quality control of mass production products.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a quality judgment method of a cast monocrystalline silicon block and an ingot casting monocrystalline silicon block, the method provides a brand-new removing mode of the head of the ingot casting monocrystalline silicon block by combining a photoluminescence testing technology with the growth characteristics of the ingot casting monocrystalline silicon ingot, the method is simple and convenient, the accuracy is high, the defects of the head of the silicon block can be effectively removed, and the quality of the removed silicon block is obviously improved.
In one aspect of the present invention, there is provided a method for judging quality of a cast single crystal silicon ingot, comprising the steps of:
(1) uniformly removing the head of the ingot casting monocrystalline silicon block by about 30-60 mm.
(2) Measuring a photoluminescence test picture of the head end face of the ingot casting monocrystalline silicon block by using a photoluminescence tester, and calculating to obtain a black silk area proportion value D of the photoluminescence test pictureS；
(3) Measuring and calculating the end surface area S of the ingot casting single crystal silicon block;
(4) establishing a black silk growth calculation model, and determining the ratio value D of the removal length L of the silicon briquette to the area of the black silk on the preset end surfaceLIs a relational expression L (D)L⍺), wherein ⍺ is the dislocation growth angle;
(5) according to the preset end face black silk area proportion value DLAnd the relation L (D)L⍺) calculating the value of the silicon block removal length L;
(6) and removing the head of the ingot casting monocrystalline silicon block according to the value of the silicon block removal length L.
An effective silicon block head removing mode is determined by constructing a black wire growth calculation model and utilizing the existing photoluminescence technology and combining the growth characteristics of dislocation of the ingot single-crystal silicon block, so that the overall quality of the ingot single-crystal silicon block is guaranteed.
Further, in the step (4), the relation L (D)L⍺) is:
wherein L is the removal length of the silicon block; s is the area of the end face of the silicon block, DSIs the area ratio of black filament on the end face of the head of the silicon block, DLThe area ratio value of the black filament at the end face of the silicon block is preset, and ⍺ is a dislocation growth angle.
Further, in the step (4), the crystal orientation of the ingot single crystal silicon block is (100), and the determined formula of the dislocation growth angle ⍺ is as follows: ⍺ =45/2v, where v is the crystal growth rate.
Alternatively, the crystal growth velocity v is calculated from the height of the original silicon ingot and the solidification time of the original silicon ingot.
Alternatively, v has a value of 0.50 to 1.2 cm/h.
Optionally, the v value of the ingot-casting monocrystalline silicon block as the central region silicon block is larger than the v value of the ingot-casting monocrystalline silicon block as the edge region silicon block or the corner region silicon block.
Further, when the ingot-cast single crystal Si ingot is a central region Si ingot, DLThe value of (A) is 15% -20%; when the ingot casting single crystal silicon block is an edge region silicon block or a corner region silicon block, DLThe value of (A) is 10 to 15%.
In another aspect of the invention, the invention discloses an ingot casting monocrystalline silicon block which is prepared by adopting any one of the judging modes of the ingot casting monocrystalline silicon block.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a flow chart of one embodiment of the present invention.
FIG. 2 is a minority carrier lifetime scan of an ingot of single crystal silicon of the present invention.
FIG. 3 is a schematic diagram of the black silk model construction of the present invention.
Fig. 4 is a black-line surface view of an ingot-casting single-crystal silicon ingot according to the first embodiment of the present invention.
FIG. 5 is a black-line surface view of an ingot-cast single-crystal silicon ingot according to a second embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In one aspect of the present invention, as shown in fig. 1, there is provided a method for judging quality of a cast single crystal silicon ingot, comprising the steps of:
(1) uniformly removing the head of the ingot casting monocrystalline silicon block by about 30-60 mm.
In the step, after an original cast ingot discharged from the furnace is cut, the head of the cast ingot monocrystalline silicon block is uniformly removed by 30-60mm, for example, 30mm, 35mm, 40mm, 45mm, 50mm, 55mm or 60 mm. Due to the segregation effect, impurities at the head of the silicon block are more, and because the ingot casting monocrystalline silicon ingot grows in a directional solidification mode, the head of the silicon block can have some obvious impurities or dirt, the areas can not be generally used for preparing a battery piece, the detection result of a photoluminescence tester can be influenced, and the head of the silicon block is uniformly removed by 30-60mm, so that the characterization of the photoluminescence test picture measured by the photoluminescence tester on the area ratio of the black wire can be more representative, and the quality of the final ingot casting monocrystalline silicon block can be further improved.
(2) Measuring a photoluminescence test picture of the head end face of the ingot casting monocrystalline silicon block by using a photoluminescence tester, and calculating to obtain a black silk area proportion value D of the photoluminescence test pictureS；
In the step, a Photoluminescence tester (PL) is a technical detection and analysis means commonly used by those skilled in the art, and is mainly used for detecting subfissure, fragments, growth defects and the like of silicon wafers, battery pieces and the like, wherein the growth defects are detected most frequently, PL test results reflect the quality conditions of surface layers of test surfaces, and crystal structure defects such as surface layer dislocation, grain boundaries and the like can be displayed. Photoluminescence test patterns measured by the photoluminescence tester are mainly shown in fig. 4 and 5, agglomerated black lines in the photoluminescence test patterns are generally called as "black filaments" (shown as circles in the left picture of fig. 4), and the black filaments are mainly considered as dislocations as known by referring to the electronic industry standard SJ/T11629-2016 "online photoluminescence analysis method of silicon wafers and battery cells for solar cells. And the photoluminescence tester can calculate to obtain a proportional value of the area of the black silk, namely the proportional value of the area of the black silk in the figure occupying the whole silicon area after setting the pixel threshold value according to the pixel difference between the black silk and the silicon background.
In the step, the photoluminescence test picture test is carried out on the head part of the monocrystalline silicon block, and the black wire area proportion value D of the photoluminescence test picture is obtained through calculationSThereby carrying out the quality judgment of the subsequent silicon blocks.
(3) Measuring and calculating the end surface area S of the ingot casting monocrystalline silicon block;
in the step, the end surface area S of the ingot single crystal silicon block can be calculated by measuring the edge width dimension of the silicon block.
It is understood that the sequence of step (1) and step (2) is not sequential, and may be simultaneous, or step (1) may be before step (2), or step (2) may be before step (1).
(4) Establishing a black silk growth calculation model, and determining the ratio value D of the removal length L of the silicon briquette to the area of the black silk on the preset end surfaceLIs a relational expression L (D)L⍺), wherein ⍺ is the dislocation growth angle;
in the step, as mentioned above, the black filament in the ingot single crystal mainly consists of dislocation, and the inventor finds that the generation of the black filament, namely the dislocation, is mainly in the preparation process of the ingot single crystal, because the mode of combining directional solidification and seed crystal splicing, bottom laying and seeding is adopted, a gap exists in the seed crystal splicing process, the dislocation is easily generated at a certain part of a silicon block in the growth process, and the dislocation has very rapid dislocation slip increment because no grain boundary barrier similar to the traditional polycrystal exists, and the dislocation is slipped and proliferated at a certain angle.
Minority carrier lifetime is also a technical detection and analysis means commonly used by those skilled in the art, and the minority carrier lifetime is mainly an index for representing metal impurities or lattice defects (grain boundaries, dislocations, and the like) inside a silicon block. The inventor further analyzes the minority carrier lifetime graph of the ingot single crystal silicon block, and finds that, referring to fig. 2, fig. 2 is a picture of the minority carrier lifetime of the side surface of the single crystal silicon block, namely the minority carrier lifetime of the silicon block from beginning to end, wherein the upper end surface is the head of the silicon block, and the lower end surface is the tail of the silicon block, and as can be seen from the figure, the straight line indicated by an arrow in the figure is that the lattice defect grows upwards from the bottom at a certain angle and diverges all around. In view of the above findings, the construction of the black filament model is based mainly on the dislocation slip propagation growth theory, the growth plane of the ingot single crystal silicon ingot is generally (100) direction, the dislocations are likely to appear in the low energy plane (111) direction, the included angle ⍺ between the (111) crystal direction and the (100) growth plane is constant, so that when the dislocations are generated under ideal conditions, the ingot single crystal silicon ingot will slip and propagate at a constant included angle ⍺, and thus the black filament theoretical model established by the inventor is shown in fig. 3, the left side is a perspective view of the black filament (i.e., dislocation) growth model, the right side is a front view of the black filament growth model, and the left side shows that the end surface area of the ingot silicon ingot is S and the black filament area ratio is DSThen, the black silk area is S × DSIf the predetermined black silk area ratio of the predetermined dislocation position is reached is DLThe black filament area is SxDLThen, the dislocation radius of the end face at this time:
dislocation radius at predetermined position:
from the right figure, Tan ⍺ = rS/ L0Wherein L is0Is the height of the ingot of single crystal silicon (i.e., the height of the ingot from the tail to the head), and rS/ rL= L0/ (L0-L), from which it follows:
L=(rS- rL) / Tan⍺ （3）
in combination with (1), (2) and (3),
wherein: l is the removal length of the silicon block; s is the area of the end face of the silicon block, DSIs the area ratio of black filament on the end face of the head of the silicon block, DLThe area ratio value of the black filament at the end face of the silicon block is preset, and ⍺ is a dislocation growth angle.
In some specific embodiments, the ingot of single crystal silicon has a crystal orientation of (100) and the determined formula for the dislocation growth angle ⍺ is: ⍺ =45/2v, where v is the crystal growth rate. The growth plane of the ingot single crystal silicon block is generally in the (100) direction, dislocations are easy to appear in the (111) direction of the low energy plane, the angle between the (111) crystal direction and the (100) growth plane is 45 degrees in an ideal case, namely, the dislocation of the silicon block slips at a dislocation angle of 45 degrees in an ideal case, ⍺ =45/2=22.5 degrees, but in practical cases, the crystal growth rate of the silicon ingot influences the dislocation angle by comparing the dislocation growth characteristics of the center of the silicon ingot and the edge of the silicon ingot, and exists in an inverse proportion relation, namely, the growth speed is smaller as the dislocation angle is larger as the growth speed is larger, and the growth speed is smaller as the growth speed is larger, specifically ⍺ =45/2v, wherein the crystal growth speed v is obtained by settling the height of the original silicon ingot and the solidification time of the original silicon ingot. In some specific embodiments, v may have a value of 0.50 to 1.20cm/h, for example 0.5 cm/h, 0.6 cm/h, 0.7 cm/h, 0.8 cm/h, 0.9cm/h, 1.0 cm/h, 1.1cm/h or 1.2 cm/h. Furthermore, in the ingot single crystal of the same furnace, the v value of the ingot single crystal silicon block as the central region silicon block is greater than the v value of the ingot single crystal silicon block as the edge region silicon block or the corner region silicon block.
(5) According to the preset end face black silk area proportion value DLAnd the relation L (D)L⍺) calculating the value of the silicon block removal length L;
in this step, the relationship L (D) is determined byL⍺) and according to D)LCan effectively calculate the value of L, and in some specific embodiments, DLMay be between 0 and 100%, preferably, DLMay be from 10% to 20%, and may for example be 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20%, when D isLWhen the value of the head silicon block is more than 20%, the efficiency of preparing the silicon wafer cut from the head silicon block into the battery piece is low, so that the reject ratio of the battery piece is high; if D isLWhen the value of (b) is less than 10%, the removal length is excessive and the cost is excessive.
Further, when the ingot of single-crystal silicon is a central-region silicon ingot, DLMay be 15% to 20%, for example 15%, 16%, 17%, 18%, 19% or 20%; when the ingot casting single crystal silicon block is an edge region silicon block or a corner region silicon block, DLValues of (b) may be 10% to 15%, for example 10%, 11%, 12%, 13%, 14%, 15%. Ingot single crystal silicon ingots are generally prepared as cubes and cut into 5 × 5=25 or 6 × 6=36 according to the subsequent size of the silicon wafer, wherein, for example, in a 5 × 5=25 silicon wafer, there are 4 corner silicon ingots, 12 edge silicon ingots and 9 center silicon ingots, the quality of the center region silicon ingots is better than that of the edge silicon ingots due to segregation of impurities and diffusion of crucible walls, and particularly, the content of impurities with small condensation coefficients such as metals is slightly lower than that of the edge and corner silicon ingots, so that the efficiency of the subsequently prepared battery is within an acceptable range even if the area ratio of black wires is slightly higher. Such a determination method can further reduce the cost.
(6) And removing the head of the ingot casting monocrystalline silicon block according to the value of the silicon block removal length L.
In this step, the removal of the head of the silicon block is performed by the L value calculated as described above.
In another aspect of the invention, the invention discloses an ingot casting monocrystalline silicon block which is prepared by adopting any one of the judging modes of the ingot casting monocrystalline silicon block.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
Selecting a silicon block in the central region of an original ingot casting single crystal with a (100) crystal orientation, and removing the head of the silicon block by 30 mm;
as shown in the left diagram of fig. 4, a photoluminescence tester is used to measure a photoluminescence picture of the head end face of the ingot single crystal silicon block, and a black silk area proportion value D of the photoluminescence picture of the head end face is calculatedS66.5 percent;
measuring and calculating the end surface area S =158 × 158 of the ingot single crystal silicon block;
the crystal growth speed is calculated to be 0.86cm/h according to the height of the silicon ingot and the solidification finishing time of the silicon block in the central area.
Setting a black silk area ratio value D of a preset end faceLIs 15.25%, and S =158 × 158, DS=66.5%, ⍺ =45/(2 × 0.86) into L (D)L⍺) is given by the following relationship:
after the head part of the silicon block is removed by 77mm, the black filament area ratio of the end face of the head part of the silicon block is measured by using a photoluminescence tester again, as shown in the right diagram of figure 4, the black filament area ratio is 15.22 percent through measurement and calculation,
example 2
Selecting a silicon block in the edge region of an original ingot single crystal with a (100) crystal direction, and removing the head of the silicon block by 50 mm;
as shown in the left diagram of fig. 5, a photoluminescence tester is used to measure a photoluminescence picture of the head end face of the ingot single crystal silicon block, and a black silk area proportion value D of the photoluminescence picture of the head end face is calculatedS84 percent;
measuring and calculating the end surface area S =158 × 158 of the ingot single crystal silicon block;
the crystal growth speed is calculated to be 0.778cm/h through the height of the silicon ingot and the solidification finishing time of the silicon block in the central area.
Setting a black silk area ratio value D of a preset end faceLIs 11.5%, and S =158 × 158, DS=84%, ⍺ =45/(2 × 0.778) into L (D)L⍺) is given by the following relationship:
and after the head part of the silicon block is removed by 93mm, measuring the area proportion of the black filaments on the end face of the head part of the silicon block by using a photoluminescence tester again, and as shown in the right diagram of fig. 5, measuring and calculating to obtain the area proportion of the black filaments to be 11.75%.
Evaluation indexes are as follows: error rate = | proportion value of black silk area of preset end face-proportion value of black silk area of actual end face |/black silk area of preset end face |)
Calculation shows that the error between the black silk area ratio value of the preset end face and the black silk area ratio value of the actual end face in the embodiment 1 and the embodiment 2 is not more than 0.3 percent, the determination method is simple and convenient, the accuracy is high, the defect of the head of the silicon block can be effectively removed, and the quality of the removed silicon block is obviously improved.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (8)
1. A quality judgment method of an ingot casting monocrystalline silicon block is characterized by comprising the following steps:
uniformly removing the head of the ingot casting monocrystalline silicon block by about 30-60 mm;
measuring a photoluminescence test picture of the head end face of the ingot casting monocrystalline silicon block by using a photoluminescence tester, and calculating to obtain a black silk area proportion value D of the photoluminescence test pictureS；
Measuring and calculating the end surface area S of the ingot casting single crystal silicon block;
establishing a black silk growth calculation model, and determining the ratio value D of the removal length L of the silicon briquette to the area of the black silk on the preset end surfaceLIs a relational expression L (D)L⍺), wherein ⍺ is the dislocation growth angle;
according to the preset end face black silk area proportion value DLAnd the relation L (D)L⍺) calculating the value of the silicon block removal length L;
and removing the head of the ingot casting monocrystalline silicon block according to the value of the silicon block removal length L.
2. The method of judging the quality of an ingot-casting single crystal silicon ingot according to claim 1, wherein in the step (4), the relational expression L (D) isL⍺) is:
wherein L is the removal length of the silicon block; s is the area of the end face of the silicon block, DSIs the area ratio of black filament on the end face of the head of the silicon block, DLThe area ratio value of the black filament at the end face of the silicon block is preset, and ⍺ is a dislocation growth angle.
3. The method for judging the quality of the ingot-cast single crystal silicon ingot according to claim 1, wherein in the step (4), the crystal orientation of the ingot-cast single crystal silicon ingot is (100), and the determination formula of the dislocation growth angle ⍺ is: ⍺ =45/2v, where v is the crystal growth rate.
4. The method of determining the quality of an ingot of single crystal silicon according to claim 3, wherein the crystal growth rate v is calculated from the height of the starting silicon ingot and the solidification time of the starting silicon ingot.
5. The method for judging the quality of an ingot-casting single-crystal silicon ingot according to claim 4, wherein the value of v is from 0.50 to 1.20 cm/h.
6. The method for judging the quality of the ingot-cast single-crystal silicon ingot according to claim 3, wherein the v value of the ingot-cast single-crystal silicon ingot as the center region silicon ingot is larger than the v value of the ingot-cast single-crystal silicon ingot as the edge region silicon ingot or the corner region silicon ingot.
7. The method for judging the quality of an ingot-casting single-crystal silicon ingot according to claim 2, wherein D is defined as a center-region silicon ingotLThe value of (A) is 15% -20%; when the ingot casting single crystal silicon block is an edge region silicon block or a corner region silicon block, DLThe value of (A) is 10 to 15%.
8. An ingot-casting single-crystal silicon ingot produced by the method for judging an ingot-casting single-crystal silicon ingot according to any one of claims 1 to 8.
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