CN118307184A - Semiconductor-grade synthetic quartz crucible and preparation method thereof - Google Patents
Semiconductor-grade synthetic quartz crucible and preparation method thereof Download PDFInfo
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- CN118307184A CN118307184A CN202410742257.8A CN202410742257A CN118307184A CN 118307184 A CN118307184 A CN 118307184A CN 202410742257 A CN202410742257 A CN 202410742257A CN 118307184 A CN118307184 A CN 118307184A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 239000010453 quartz Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000006004 Quartz sand Substances 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 50
- 238000002844 melting Methods 0.000 claims abstract description 48
- 230000008018 melting Effects 0.000 claims abstract description 48
- 238000001816 cooling Methods 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000465 moulding Methods 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims description 46
- 238000010309 melting process Methods 0.000 claims description 14
- 239000004576 sand Substances 0.000 claims description 14
- 239000004065 semiconductor Substances 0.000 claims description 13
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims 3
- 230000004927 fusion Effects 0.000 abstract description 14
- 239000012535 impurity Substances 0.000 abstract description 8
- 230000000052 comparative effect Effects 0.000 description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 229910002804 graphite Inorganic materials 0.000 description 14
- 239000010439 graphite Substances 0.000 description 14
- 239000013078 crystal Substances 0.000 description 6
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 238000007599 discharging Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a preparation method of a semiconductor-grade synthetic quartz crucible, which comprises the following steps: sequentially carrying out exhaust treatment, envelope treatment, transparent layer melting, bubble layer melting and cooling on the quartz crucible after quartz sand molding; in the processes of envelope treatment, transparent layer fusion and bubble layer fusion, the distance between the water cooling plate and the die opening is 50-80 mm. The preparation method effectively reduces the entry of external impurities, reduces the influence of the external environment on the internal melting environment of the crucible, and improves the problem of high purity of the inner surface of the R angle of the synthetic quartz crucible.
Description
Technical Field
The invention belongs to the field of monocrystalline silicon preparation, and relates to a semiconductor-grade synthetic quartz crucible and a preparation method thereof.
Background
Monocrystalline silicon as a starting material for the manufacture of most semiconductor electronic components is generally prepared by the so-called czochralski method ("CZ"). Most single crystal silicon is manufactured by the CZ method. The CZ method is a method in which a polycrystalline silicon raw material is melted in a silica glass crucible to form a silicon melt, a seed crystal is immersed in the silicon melt, and the seed crystal is slowly pulled up while rotating the silica glass crucible and the seed crystal, whereby a large single crystal is grown at the lower end of the seed crystal.
The crucibles used in conventional crystal pulling are generally composed of quartz because of its purity, temperature stability and chemical resistance. In order to obtain the high-purity monocrystalline silicon rod, researchers change the natural high-purity quartz sand on the inner surface into artificial synthetic quartz sand with higher purity, but the synthetic sand has low viscosity and cannot be used in full proportion, and the outer layer needs to be made of the natural high-purity quartz sand with higher strength as a support; and the synthetic quartz sand has high price and high cost. When the synthetic quartz crucible is prepared, only 2-3mm synthetic sand is added to the inner surface of the synthetic quartz crucible. Thus, the purity of the inner surface of the crucible is ensured, and the cost is reduced. Since impurities induce crystallization of quartz sand, the purity of the inner surface of the crucible is one of the most important indexes for evaluating a synthetic quartz crucible.
In the preparation process of the synthetic quartz crucible, the impurity content of the inner surface of the crucible cannot be effectively controlled due to more factors of external influence. Moreover, during the preparation process, the bottom quartz sand moves due to the melting process, so that part of the outer natural sand enters the inner surface of the crucible, and the purity of the inner surface of the crucible is reduced. Japanese patent JP 2004518601A: through a semi-closed type melting device, the air in the melting area of the crucible is replaced by introducing 'reactive' gas, so that the expected atmosphere is achieved, and the melting environment of the quartz crucible is improved.
In the prior art, when a synthetic quartz crucible is prepared by a quartz crucible vacuum arc method, the purity of the inner surface of the crucible is influenced by external impurities in the melting process. Because the synthetic quartz sand on the inner surface only uses a small part when the synthetic crucible is prepared, the main viscosity is low and the price is high, the R angle and the bottom purity can be greatly reduced because the original basic process has small opening and closing, large impact and large movement and the sand mixing probability can be increased.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a semiconductor-grade synthetic quartz crucible and a preparation method thereof, wherein the preparation method effectively reduces the entry of external impurities, reduces the influence of the external environment on the melting environment in the crucible, and improves the problem of high purity of the inner surface of an R angle of the synthetic quartz crucible.
In order to achieve the technical effects, the invention adopts the following technical scheme:
One of the objects of the present invention is to provide a method for preparing a semiconductor grade synthetic quartz crucible, comprising:
Sequentially carrying out exhaust treatment, envelope treatment, transparent layer melting, bubble layer melting and cooling on the quartz crucible after quartz sand molding;
in the processes of envelope treatment, transparent layer fusion and bubble layer fusion, the distance between the water cooling plate and the die opening is 50-80 mm.
The distance between the water cooling plate and the die opening may be 50mm, 55 mm, 60mm, 65 mm, 70 mm, 75 mm, 80 mm, or the like, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
As a preferable technical scheme of the invention, in the quartz sand molding, the natural high-purity quartz sand used at the R angle and the bottom is natural high-purity quartz sand IOTA-6.
As a preferable technical scheme of the invention, the mixed gas of the simple substance gas and the oxygen is introduced into the exhaust treatment and vacuumized, and the density of the simple substance gas is less than that of air.
As a preferable technical scheme of the invention, the volume fraction of the simple substance gas in the mixed gas is 80-90%, and the volume fraction of the oxygen is 10-20%. The volume fraction of the elemental gas may be 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, or the like, and the volume fraction of the oxygen may be 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, or the like, but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned respective ranges are equally applicable.
Preferably, the elemental gas comprises an inert gas.
As a preferable technical scheme of the invention, the introducing rate of the mixed gas is 0.25-0.5 MPa/min, such as 0.25-MPa/min, 0.3-MPa/min, 0.35-MPa/min, 0.4-MPa/min, 0.45-MPa/min or 0.5-MPa/min, etc., but the mixed gas is not limited to the listed values, and other non-listed values in the range of the values are applicable.
In the cover treatment, the electrodes are opened and closed by 20 to 35 mm, such as 20mm, 22 mm, 25 mm, 28 mm, 30 mm, 32 mm or 35 mm, but the invention is not limited to the above-mentioned values, and other non-mentioned values are applicable in the above-mentioned range.
Preferably, the envelope is treated with a gas mixture and a vacuum is applied.
In a preferred embodiment of the present invention, the electrodes are opened and closed at 45 to 55 mm, for example, 45 mm, 46 mm, 47 mm, 48 mm, 49 mm, 50 mm, 51 mm, 52 mm, 53 mm, 54 mm or 55 mm, etc., but the present invention is not limited to the above-mentioned values, and other non-mentioned values are applicable within the above-mentioned values.
Preferably, during the transparent layer melting, the mixed gas is kept to be introduced and vacuumized.
In a preferred embodiment of the present invention, the electrodes are opened and closed by 35 to 45 mm in the bubble layer melting, for example, 35 mm, 36 mm, 37 mm, 38 mm, 39 mm, 40 mm, 41 mm, 42 mm, 43 mm, 44 mm or 45 mm, etc., but the present invention is not limited to the above-mentioned values, and other non-mentioned values in the above-mentioned numerical ranges are applicable.
Preferably, in the bubble layer melting, the mixed gas is stopped from being introduced and vacuumized.
The second object of the invention is to provide a semiconductor grade synthetic quartz crucible prepared by the method for preparing the semiconductor grade synthetic quartz crucible provided by one of the objects.
The third object of the present invention is to provide a semiconductor grade single crystal silicon growing method using the semiconductor grade synthetic quartz crucible provided in the second object.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) The invention provides a semiconductor-grade synthetic quartz crucible and a preparation method thereof, wherein the preparation method improves relative heat to a certain extent by reducing the height of a water cooling plate, and solves the problem that microbubbles on the R-angle surface of a 32-inch synthetic crucible cannot be removed;
(2) The invention provides a semiconductor-grade synthetic quartz crucible and a preparation method thereof, wherein the preparation method reduces the entry of external impurities and the influence of the external world on the melting environment in the crucible by reducing the height of a water cooling plate;
(3) The invention provides a semiconductor-grade synthetic quartz crucible and a preparation method thereof, which solve the problems that the bottom synthetic sand is impacted and the purity of the inner surface is reduced due to the small opening and closing of an electrode, low electrode position and the impact of arc light on the bottom quartz sand;
(4) The invention provides a semiconductor-grade synthetic quartz crucible and a preparation method thereof, and the preparation method solves the problem that the purity of the inner surface of an R angle of the existing synthetic quartz crucible is high.
Drawings
FIG. 1 is a schematic view showing an apparatus used in a method for manufacturing a semiconductor grade synthetic quartz crucible according to an embodiment of the present invention;
In the figure: 1 is a high-purity graphite electrode; 2 is a mixed gas vent pipe; 3 is a graphite mold vacuumizing hole; 4 is a graphite mold; 5 is a quartz crucible bubble layer; 6 is a transparent layer on the inner surface of the quartz crucible; 7 is a transparent layer straight wall of the quartz crucible; 8 is the R angle and the bottom of the transparent layer of the quartz crucible; 9 is a water cooling plate; and 10 is exhaust air.
The present invention will be described in further detail below. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims.
Detailed Description
The technical scheme of the application is further described through the specific embodiments.
The embodiment of the invention provides a preparation method of a semiconductor-grade synthetic quartz crucible, which comprises the following steps:
Sequentially carrying out exhaust treatment, envelope treatment, transparent layer melting, bubble layer melting and cooling on the quartz crucible after quartz sand molding;
in the processes of envelope treatment, transparent layer fusion and bubble layer fusion, the distance between the water cooling plate and the die opening is 50-80 mm.
In one specific embodiment of the invention, an exhaust assembly is arranged above the water cooling plate.
Because the existing melting process has a distance of 150-300 mm from the position of the die opening in the preparation process, the influence of external impurities on the inside of the crucible in the melting process is improved by a higher distance. According to the invention, the distance between the water cooling plate and the quartz sand is reduced to 50-80 mm, and air in the gap between the mixed gas replacement die and the quartz sand is filled, so that the melting atmosphere of the quartz crucible is improved, and the influence of external impurities on the inner surface of the crucible is greatly reduced. The air exhaust component above the water cooling plate also reduces the influence of external factors, and the air exhaust component also pumps away ash generated in the melting process of the graphite electrode. And a certain amount of white quartz plates formed by gasification and cooling under the high-temperature condition of quartz sand are removed. So that the method is similar to a semi-closed synthetic crucible melting preparation process.
For a 32-inch synthetic quartz crucible, the outer diameter of the 32-inch synthetic quartz crucible is larger, so that heat loss is too fast in the process of preparation, and the heat is insufficient, so that the difficulty in preparing the 32-inch synthetic crucible is increased. According to the invention, under the condition that the original basic process is not changed, the position of the water cooling plate is reduced and adjusted, so that the heat in the melting process is improved to a certain extent, and the ablation of transparent layer microbubbles of the synthetic quartz crucible is effectively improved.
In one embodiment of the invention, the quartz sand molding method can be as follows:
The first step: transferring the melting rotary die for 45-56 degrees, rotating at 65-70 rpm, pouring natural quartz sand (70-140 meshes) on the outer surface into the die, and then forming straight-wall natural high-purity quartz sand by using a forming rod;
A second part: the melting rotary die is transposed by 0 DEG, the rotating speed is 65-70 rpm, and a forming rod is used for scraping off natural high-purity quartz sand of a straight wall part to enable the quartz sand to fall into the bottom until the forming of the outer surface of the whole crucible is completed;
and a third step of: forming a straight wall by using part of the synthetic quartz sand by using a forming machine until the straight wall is formed;
fourth step: and finally, manually forming the bottom and the R angle part, and remaining synthetic quartz sand until the final forming is finished.
In one specific embodiment of the invention, in quartz sand molding, the natural high-purity quartz sand used for the R angle and the bottom is natural high-purity quartz sand IOTA-6.
In the invention, natural high-purity quartz sand NC4A with synthetic sand removed from the bottom and R-angle transparent layer is replaced by IOTA-6 with higher purity. Because the bottom can inevitably cause a part of mixed materials under the action of centrifugal force in the melting process, the transparent layer part except the synthetic sand at the bottom and the R angle is replaced by IOTA-6 sand with higher purity, so that the influence of the IOTA-6 sand is reduced as much as possible. Multiple shots of synthetic sand, although one way, are low in viscosity, can result in reduced bottom strength, and are expensive.
In one specific embodiment of the invention, mixed gas consisting of simple substance gas and oxygen is introduced into the mold, so that air in the mold and air in a quartz sand gap are removed as much as possible, and the time can be 3-4 min.
In a specific embodiment of the invention, vacuum is pumped in the exhaust treatment process, and the vacuum pressure is 0 to-0.99 MPa.
In one embodiment of the present invention, the inert gas in the mixed gas used in the exhaust treatment may be helium, argon, or the like.
In a specific embodiment of the invention, in envelope treatment, open layer fusion and bubble layer fusion, the opening and closing of the electrodes are increased by 20-30% compared with the original process.
In the invention, as the original process electrode is small in opening and closing, the synthetic sand at the bottom of the inner part of the mold is impacted, so that the R angle and the bottom are mixed with part of natural high-purity quartz sand, and the purity of the inner surface of the crucible is affected. In the invention, in order to improve the impact of the arc on the bottom quartz sand in the melting process, the impact of the arc on the bottom synthetic quartz sand can be effectively improved by increasing the opening and closing of the electrode in a reasonable range, so that the problem of high R-angle purity of the synthetic quartz crucible caused by the impact is greatly avoided, and the straight wall generally moves relatively less under the action of centrifugal force.
In a specific embodiment of the invention, in the envelope treatment, the arc striking power of the graphite electrode is 10-15 kW.
In one specific embodiment of the invention, in the cover treatment, the mixed gas is kept to be introduced, and the introducing speed of the mixed gas is 0.25-0.5 MPa/min.
In one specific embodiment of the invention, in the cover treatment, vacuum is maintained, and the vacuum pressure is 0 to-0.99 MPa.
In one embodiment of the present invention, the time for processing the cover may be 1-2 minutes.
In a specific embodiment of the invention, the power of the graphite electrode in the transparent layer melting is 25-30 kW.
In one specific embodiment of the invention, the mixed gas is kept to be introduced in the transparent layer melting process, and the introducing rate of the mixed gas is 0.25-0.5 MPa/min.
In one specific embodiment of the invention, vacuum is maintained in the process of melting the transparent layer, and the vacuum pressure is 0 to-0.99 MPa.
In one embodiment of the present invention, the time for melting the transparent layer may be 3 to 4 minutes.
In one specific embodiment of the invention, the power of the graphite electrode is 16-20 kW in the bubble layer melting process.
In one embodiment of the invention, the time for melting the bubble layer may be 6-10 min.
In one specific embodiment of the invention, the graphite arc is closed before cooling, and kept for 5-8 min until the inner surface of the crucible is cooled, and then the crucible is discharged, demoulded and melted.
In one embodiment of the present application, in the semiconductor grade single crystal silicon growing method, except for using the semiconductor grade synthetic quartz crucible provided by the present application, the other conditions can be appropriately adjusted according to the single crystal silicon growing method commonly used in the art, and are not further limited herein.
For a better illustration of the present invention, which is convenient for understanding the technical solution of the present invention, exemplary but non-limiting examples of the present invention are as follows:
example 1
The present embodiment provides a method for manufacturing a semiconductor-grade synthetic quartz crucible, the method comprising:
Sequentially carrying out exhaust treatment, envelope treatment, transparent layer melting, bubble layer melting and cooling on the quartz crucible after quartz sand molding;
in the processes of envelope treatment, transparent layer fusion and bubble layer fusion, the distance between the water cooling plate and the die opening is 50 mm;
In the exhaust treatment, mixed gas of helium (volume fraction 80%) and oxygen (volume fraction 20%) is introduced and vacuumized, and the density of the simple substance gas is less than that of air;
In the envelope treatment, the graphite electrode is started to be arc, and the mixed gas is kept to be introduced and vacuumized;
In the transparent layer melting process, the mixed gas is kept to be introduced and vacuumized;
In the process of melting the bubble layer, stopping introducing mixed gas and vacuumizing;
closing the graphite arc before cooling, and rapidly cooling the quartz crucible;
and after cooling, discharging from the furnace, demoulding and melting.
The conditions of each step in example 1 are shown in Table 1.
TABLE 1
Example 2
The present embodiment provides a method for manufacturing a semiconductor-grade synthetic quartz crucible, the method comprising:
Sequentially carrying out exhaust treatment, envelope treatment, transparent layer melting, bubble layer melting and cooling on the quartz crucible after quartz sand molding;
in the processes of envelope treatment, transparent layer fusion and bubble layer fusion, the distance between the water cooling plate and the die opening is 80 mm;
In the exhaust treatment, mixed gas of helium (volume fraction 90%) and oxygen (volume fraction 10%) is introduced and vacuumized, and the density of the simple substance gas is less than that of air;
In the envelope treatment, the graphite electrode is started to be arc, and the mixed gas is kept to be introduced and vacuumized;
In the transparent layer melting process, the mixed gas is kept to be introduced and vacuumized;
In the process of melting the bubble layer, stopping introducing mixed gas and vacuumizing;
closing the graphite arc before cooling, and rapidly cooling the quartz crucible;
and after cooling, discharging from the furnace, demoulding and melting.
The conditions of each step in example 2 are shown in Table 2.
TABLE 2
Example 3
The present embodiment provides a method for manufacturing a semiconductor-grade synthetic quartz crucible, the method comprising:
Sequentially carrying out exhaust treatment, envelope treatment, transparent layer melting, bubble layer melting and cooling on the quartz crucible after quartz sand molding;
In the processes of envelope treatment, transparent layer fusion and bubble layer fusion, the distance between the water cooling plate and the die opening is 65 mm;
in the exhaust treatment, mixed gas of helium (volume fraction 85%) and oxygen (volume fraction 15%) is introduced and vacuumized, and the density of the simple substance gas is less than that of air;
In the envelope treatment, the graphite electrode is started to be arc, and the mixed gas is kept to be introduced and vacuumized;
In the transparent layer melting process, the mixed gas is kept to be introduced and vacuumized;
In the process of melting the bubble layer, stopping introducing mixed gas and vacuumizing;
closing the graphite arc before cooling, and rapidly cooling the quartz crucible;
and after cooling, discharging from the furnace, demoulding and melting.
The conditions of each step in example 3 are shown in Table 3.
TABLE 3 Table 3
Example 4
In this example, the conditions were the same as in example 3 except that the distance between the water-cooling plate and the die opening was 60 mm.
Example 5
In this example, the conditions were the same as in example 3 except that the distance between the water-cooling plate and the die opening was 75 mm.
The method of the quartz sand molding stage in examples 1 to 5 is as follows:
The first step: transferring the melting rotary die for 45-56 degrees, rotating at 65-70 rpm, pouring natural quartz sand (70-140 meshes) on the outer surface into the die, and then forming straight-wall natural high-purity quartz sand by using a forming rod;
A second part: the melting rotary die is transposed by 0 DEG, the rotating speed is 65-70 rpm, and a forming rod is used for scraping off natural high-purity quartz sand of a straight wall part to enable the quartz sand to fall into the bottom until the forming of the outer surface of the whole crucible is completed;
and a third step of: forming a straight wall by using part of the synthetic quartz sand by using a forming machine until the straight wall is formed;
fourth step: and finally, manually forming the bottom and the R angle part, and remaining synthetic quartz sand until the final forming is finished.
The apparatus of the method for manufacturing a semiconductor grade synthetic quartz crucible provided in examples 1 to 5 is shown in FIG. 1, wherein the bubble layer uses natural high purity quartz sand NC4A, the transparent layer on the inner surface of the quartz crucible uses synthetic quartz sand, the transparent layer straight wall of the quartz crucible uses natural high purity quartz sand NC4A, and the corners and bottom of the transparent layer R of the quartz crucible use natural high purity quartz sand IOTA-6.
Comparative example 1
In this comparative example, the conditions were the same as in example 3 except that the distance between the water-cooling plate and the die opening was 150 mm.
Comparative example 2
In this comparative example, the conditions were the same as in example 3 except that the distance between the water-cooling plate and the die opening was 300 mm.
Comparative example 3
In this comparative example, the conditions were the same as in example 3 except that the electrode was opened and closed at 16.7 mm in the envelope treatment.
Comparative example 4
In this comparative example, the conditions were the same as in example 3 except that the electrode was opened and closed at 37.5 mm in the transparent layer melting.
Comparative example 5
In this comparative example, the conditions were the same as in example 3 except that the opening and closing of the electrode was 29.2 mm in the bubble layer melting.
Comparative example 6
In this comparative example, the same conditions as in example 3 were followed except that the quartz crucible transparent layer R angle and the bottom were used with natural high purity quartz sand NC 4A.
TABLE 4 Table 4
The 32-inch synthetic quartz crucible was prepared by the preparation methods provided in examples 1 to 5 and comparative examples 1 to 6, and the R-angle purity of the prepared 32-inch synthetic quartz crucible was tested, and the results are shown in table 4.
The testing method of the R angle purity comprises the following steps: taking a sample synthetic quartz crucible R angle sample block, etching a 20 mu m layer on the inner surface of the R angle by using 25% HF acid, performing ICP detection on the obtained sample solution, and performing corresponding concentration conversion after no abnormality exists in comparison data, thereby obtaining the purity (ppm) of the inner surface of the quartz crucible R angle.
As can be seen from the test results of Table 4, the purity of the R-angle part of the 32-inch synthetic quartz crucible prepared by the preparation method of the semiconductor-grade synthetic quartz crucible provided by the embodiments 1-5 is high, and the influence of quartz sand crystallization on the quality of monocrystalline silicon in the growth process of the monocrystalline silicon is avoided. The distances between the water-cooled plates and the die openings in comparative examples 1 and 2 were 150 mm and 300 mm, respectively, resulting in a significant decrease in the purity of the R-angle portion as compared with example 3. In the envelope treatment in comparative example 3, the electrode opening and closing were 16.7 mm, in the transparent layer melting in comparative example 4, the electrode opening and closing were 37.5: 37.5 mm, and in the bubble layer melting in comparative example 5, the electrode opening and closing were 29.2: 29.2 mm, and the purity of the R-angle portion was slightly lowered as compared with example 3. In comparative example 6, natural high purity quartz sand NC4A was used for the R angle and bottom of the transparent layer of the quartz crucible, and the purity of the R angle portion was significantly lowered as compared with example 3.
The applicant states that the detailed structural features of the present invention are described by the above embodiments, but the present invention is not limited to the above detailed structural features, i.e. it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (10)
1. A method for preparing a semiconductor grade synthetic quartz crucible, the method comprising:
Sequentially carrying out exhaust treatment, envelope treatment, transparent layer melting, bubble layer melting and cooling on the quartz crucible after quartz sand molding;
in the processes of envelope treatment, transparent layer melting and bubble layer melting, the distance between the water cooling plate and the die opening is 50-80 mm.
2. The method according to claim 1, wherein the natural high purity silica sand used for the R-angle and the bottom in the silica sand molding is natural high purity silica sand IOTA-6.
3. The method according to claim 1, wherein the exhaust treatment is performed by introducing a mixed gas of an elemental gas having a density smaller than that of air and oxygen and evacuating.
4. The preparation method of claim 3, wherein the volume fraction of the simple substance gas in the mixed gas is 80-90%, and the volume fraction of the oxygen is 10-20%;
the elemental gas includes an inert gas.
5. The method according to claim 3, wherein the rate of introducing the mixed gas is 0.25 to 0.5 MPa/min.
6. The method according to claim 3, wherein in the cover treatment, the opening and closing of the electrodes are 20 to 35 mm;
in the envelope treatment, the mixed gas is kept to be introduced and vacuumized.
7. The method according to claim 3, wherein the electrode is opened or closed by 45 to 55 mm in the melting of the transparent layer;
And in the transparent layer melting process, the mixed gas is kept to be introduced and vacuumized.
8. The method according to claim 3, wherein the opening and closing of the electrodes is 35 to 45 mm in the melting of the bubble layer;
And stopping the mixed gas from being introduced and vacuumizing in the process of melting the bubble layer.
9. A semiconductor grade synthetic quartz crucible, characterized in that it is produced by the method for producing a semiconductor grade synthetic quartz crucible according to any of claims 1 to 8.
10. A semiconductor-grade single crystal silicon growing method, characterized in that the semiconductor-grade single crystal silicon growing method uses the semiconductor-grade synthetic quartz crucible according to claim 9.
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| CN202410742257.8A CN118307184B (en) | 2024-06-11 | 2024-06-11 | Semiconductor-grade synthetic quartz crucible and preparation method thereof |
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| CN202410742257.8A CN118307184B (en) | 2024-06-11 | 2024-06-11 | Semiconductor-grade synthetic quartz crucible and preparation method thereof |
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| CN118307184B CN118307184B (en) | 2024-08-09 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002068841A (en) * | 2000-08-29 | 2002-03-08 | Mitsubishi Material Quartz Kk | High purity carbon electrode for arc melting |
| CN101085696A (en) * | 2006-07-05 | 2007-12-12 | 上海新沪玻璃有限公司 | Production instrument for electric arc coating quartz glass crucible and manufacturing technique thereof |
| CN111592211A (en) * | 2020-05-29 | 2020-08-28 | 锦州万得机械装备有限公司 | Large-size quartz crucible melting equipment |
| EP3951023A1 (en) * | 2020-08-04 | 2022-02-09 | Zhejiang Jinko Solar Co., Ltd. | Method and apparatus for manufacturing monocrystalline silicon |
| CN220012462U (en) * | 2023-06-20 | 2023-11-14 | 宁夏鑫晶新材料科技有限公司 | Water cooling plate structure |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002068841A (en) * | 2000-08-29 | 2002-03-08 | Mitsubishi Material Quartz Kk | High purity carbon electrode for arc melting |
| CN101085696A (en) * | 2006-07-05 | 2007-12-12 | 上海新沪玻璃有限公司 | Production instrument for electric arc coating quartz glass crucible and manufacturing technique thereof |
| CN111592211A (en) * | 2020-05-29 | 2020-08-28 | 锦州万得机械装备有限公司 | Large-size quartz crucible melting equipment |
| EP3951023A1 (en) * | 2020-08-04 | 2022-02-09 | Zhejiang Jinko Solar Co., Ltd. | Method and apparatus for manufacturing monocrystalline silicon |
| CN220012462U (en) * | 2023-06-20 | 2023-11-14 | 宁夏鑫晶新材料科技有限公司 | Water cooling plate structure |
Non-Patent Citations (1)
| Title |
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| 王玉臣: "直拉法单晶硅生长的数值模拟和控制参数优化", 《电子工业专用设备》, vol. 44, no. 07, 31 December 2015 (2015-12-31), pages 13 - 17 * |
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| CN118307184B (en) | 2024-08-09 |
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