CN116815296A - Impurity compensation doping process in crystal growth process of Czochralski method - Google Patents
Impurity compensation doping process in crystal growth process of Czochralski method Download PDFInfo
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- CN116815296A CN116815296A CN202310792282.2A CN202310792282A CN116815296A CN 116815296 A CN116815296 A CN 116815296A CN 202310792282 A CN202310792282 A CN 202310792282A CN 116815296 A CN116815296 A CN 116815296A
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- 239000013078 crystal Substances 0.000 title claims abstract description 114
- 238000000034 method Methods 0.000 title claims abstract description 104
- 239000012535 impurity Substances 0.000 title claims abstract description 43
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 230000000295 complement effect Effects 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 3
- 239000000155 melt Substances 0.000 claims description 9
- 230000000153 supplemental effect Effects 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 description 15
- 229910052732 germanium Inorganic materials 0.000 description 10
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 9
- 229910052787 antimony Inorganic materials 0.000 description 8
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 8
- 239000002019 doping agent Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000010899 nucleation Methods 0.000 description 4
- 229910001750 ruby Inorganic materials 0.000 description 3
- 239000010979 ruby Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- HZXMRANICFIONG-UHFFFAOYSA-N gallium phosphide Chemical compound [Ga]#P HZXMRANICFIONG-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 229910001751 gemstone Inorganic materials 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
Classifications
-
- 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
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
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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 application provides an impurity complementary doping process in the crystal growth process of a Czochralski method, which comprises the following steps of: a, discharging the shoulder through cooling or reserving the shoulder after crystal remelting; lifting the shoulder to a first preset height, and waiting for a first preset time to cool the shoulder; c, lowering the crystal, enabling the edge of the shoulder to be below the liquid level, rotating the crucible, stabilizing the crystal for a second preset time, lifting the shoulder to the liquid level, observing whether a step-shaped groove appears on the shoulder or not, and repeating the step B, C if the step-shaped groove does not appear on the shoulder; d, closing the crucible rotation and the crystal rotation, lifting the shoulder to the auxiliary chamber of the single crystal furnace, closing a gate valve between the main chamber and the auxiliary chamber, and waiting for a third preset time to cool the shoulder; e, opening the auxiliary chamber, and putting the impurities to be doped into the step-shaped groove; and F, closing the auxiliary chamber, evacuating, opening the gate valve, and lowering the shoulder below the liquid level to perform melting and doping.
Description
Technical Field
The application belongs to the technical field of crystal production, and particularly relates to an impurity complementary doping process in a crystal growth process of a Czochralski method.
Background
The Czochralski method is a method of pulling a single crystal from a melt using a seed crystal. Single crystals used in modern technologies such as electronics and optics, such as silicon (Si), germanium (Ge), gallium arsenide (GaAs), gallium phosphide (GaP), indium phosphide (InP), ruby, white ruby, yttrium aluminum garnet, spinel, and certain alkali and alkaline earth halides, can be grown by the czochralski method. The specific growth method is as follows: heating and melting raw materials in a crucible of a growth furnace by using the growth furnace; an end of a thin single crystal (called a seed crystal) cut into a specific crystal orientation is immersed in the melt and made slightly molten. Then, the temperature is controlled to slowly raise the seed crystal vertically, and the pulled liquid solidifies into a single crystal. The heating power is adjusted to obtain the required diameter of the single crystal rod. Doping of the crystal with impurity elements is generally required before the crystal is grown to control the electrical and optical properties of the crystal.
Taking germanium crystal growth as an example, the resistivity of the germanium lens is directly related to the infrared transmittance, the N-type antimony element is doped in the high-purity germanium through accurate calculation before the germanium crystal grows, and the resistivity of the grown crystal is controlled within 5-30Ω & cm, so that the absorption coefficient is reduced, and the infrared transmittance is increased. The segregation coefficient of antimony is less than 1 and is 0.023, so that the concentration of antimony solute in the crystal growth process is gradually increased along the axial direction, and the resistivity of the crystal is gradually reduced from beginning to end. In the process of charging or crystal growth, P-type impurities are inevitably carried in, so that the head of the crystal is compensated, and the head of the crystal is out of the resistivity range. In addition, some users need crystals with specific resistivity of 20-40, 25-40, 5-15 ohm cm and the like, and the heads of the crystals are more easily compensated by other impurities due to the smaller doping amount of antimony, so that the heads of the crystals are beyond the resistivity range. Once doping is completed before the growth of the germanium crystal is started, the doping cannot be performed again after the growth of the germanium crystal is started to adjust the resistivity. In order to meet the resistivity requirement, the length of a single crystal is often required to be shortened or a certain length is cut off at the head of the crystal, and even more, the whole crystal is scrapped, so that the production cost is greatly increased and the production efficiency is restricted.
At present, in the actual production of germanium crystals, the furnace is usually stopped for doping and re-pulling, a U-shaped accommodating cavity is drilled on the side surface of a seed crystal to accommodate antimony dopants, or a high-purity graphite device with a floating sphere is adopted to accommodate antimony dopants, and then the dopants are lowered below the liquid level of a melt to realize melting and doping.
In the first doping supplementing mode, the doping amount is recalculated after the furnace is stopped, and the furnace is opened for drawing after doping supplementing, so that the production cost is greatly increased, and the production efficiency is reduced.
The latter two modes of doping will melt the drawn crystal back, raise the seed chuck to the auxiliary chamber, cool and take out the crystal, replace the seed crystal or high purity graphite device containing antimony, evacuate and then lower the liquid level of the melt to carry out doping. After the high-purity graphite device is doped, the high-purity graphite device is required to be lifted to an auxiliary chamber again, taken out after being cooled, replaced by a new seed crystal, pumped out and then lowered below the liquid level of the melt to start seeding growth. The operation process is loaded down with trivial details, the cycle is long, especially seed crystal boring mode, holds the chamber darker, insufficient when corroding, introduces new impurity easily, leads to resistivity anomaly, and when boring, easily leads to the seed crystal to appear cleavage line, has the crystal risk that drops when crystal growth. In addition, the high-purity graphite is doped in the device, in the long-term exposure air, moisture and impurities in the air can pollute the high-purity graphite device, when the high-purity graphite device is lowered to the liquid level of the molten liquid, an oxidation film can appear on the liquid level of the molten liquid, the crystal pulling is affected, and meanwhile the risk of bringing new impurities is also caused.
Disclosure of Invention
The embodiment of the application provides an impurity complementary doping process in the crystal growth process of a Czochralski method, and aims to provide an impurity complementary doping process which is low in production cost, high in production efficiency and greatly reduces the risk of bringing in new impurities.
In order to achieve the above purpose, the application adopts the following technical scheme: the impurity complementary doping process in the crystal growth process of the Czochralski method comprises the following steps:
a, discharging the shoulder through cooling or reserving the shoulder after crystal remelting;
lifting the shoulder to a first preset height, and waiting for a first preset time to cool the shoulder;
c, lowering the crystal, enabling the edge of the shoulder to be below the liquid level, giving crucible rotation, crystal rotation, stabilizing for a second preset time, then lifting the shoulder to the liquid level, observing whether a step-shaped groove appears on the shoulder, and repeating the step B, C if the step-shaped groove does not appear; if the step-shaped groove appears, entering the next step;
d, closing the crucible rotation and the crystal rotation, lifting the shoulder to the auxiliary chamber of the single crystal furnace, closing a gate valve between the main chamber and the auxiliary chamber, and waiting for a third preset time to cool the shoulder;
e, opening the auxiliary chamber, and putting impurities to be doped into the step-shaped groove;
and F, closing the auxiliary chamber, evacuating, opening the gate valve, and lowering the shoulder to below the liquid level to perform melting and doping.
In one possible implementation of the impurity doping process in the crystal growth process of the Czochralski method provided by the application, in the step A, the shoulder is lifted at a speed of 4-6 mm/S.
In one possible implementation manner of the impurity complementary doping process in the crystal growth process of the Czochralski method provided by the application, in the step B, the shoulder is lifted in two to three first preset stages, the total lifting height is the first preset height, the first preset height is 50-60 cm, and the first preset time is 5-10 min; wherein, lifting by 20-30 cm, cooling for 1-3 min is used as a first preset stage; the lifting speed and the lifting condition can effectively avoid unexpected cracking of the shoulder caused by rapid lifting and cooling.
In one possible implementation manner of the impurity complementary doping process in the crystal growth process of the Czochralski method provided by the application, in the step C, the shoulder edge is lowered to 1-3 mm below the liquid level of the melt at a speed of 6-8 mm/S, the crucible is turned to 0.5-2 r/min, the crystal is turned to 5-10 r/min, and the second preset time is 1-3 min; the process conditions of crystal rotation and crucible rotation can enable the step-shaped grooves to be uniformly distributed around the shoulder, and the situation that the shoulder is rapidly grown to be in a sheet shape and cannot grow out of the step-shaped grooves is avoided.
In one possible implementation manner of the impurity complementary doping process in the crystal growth process of the Czochralski method, in the step D, the shoulder is lifted into the auxiliary chamber in three to four second preset stages at a speed of 4 to 6mm/S, and the third preset time is 10 to 15min; wherein, lifting by 15-20 cm, and cooling for 1-3 min is used as the second preset stage.
In one possible implementation of the impurity doping process in the crystal growth process of the Czochralski method provided by the application, in the step F, the shoulder is lowered to be below the liquid level at a speed of 6-8 mm/S for melting and doping.
The impurity complementary doping process in the crystal growth process of the Czochralski method has the beneficial effects that: compared with the prior art, the impurity complementary doping process in the crystal growth process of the Czochralski method can carry out doping at any stage of seeding, shouldering, isodiametric and the like of single crystal growth, avoids risks of shortening the pulling length, cutting off a certain length of the head part of the crystal or scrapping the whole root or re-opening the furnace for drawing and the like caused by improper initial doping, greatly saves the production cost and improves the production efficiency; meanwhile, the process does not involve the introduction of an external device and the transformation of seed crystals, so that the risk of secondary impurity pollution is avoided greatly.
Drawings
FIG. 1 is a schematic diagram of a front view structure of a shoulder portion which is cooled and released during seeding or a shoulder portion which remains after crystal remelting in an impurity complementary doping process in a crystal growth process according to an embodiment of the present application;
FIG. 2 is a schematic diagram of a front view of a shoulder portion with a stepped groove formed by an impurity doping process in a crystal growth process according to an embodiment of the present application;
FIG. 3 is a flow chart of a process for impurity doping during crystal growth in the Czochralski method according to an embodiment of the present application;
reference numerals illustrate:
10. a shoulder; 20. a stepped groove.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The following description of the technical solutions according to the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, but not all embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the application, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
The relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present application unless it is specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective parts shown in the drawings are not drawn in actual scale for convenience of description. Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further discussion thereof is necessary in subsequent figures.
In the description of the present application, it should be understood that the azimuth or positional relationships indicated by the azimuth terms such as "front, rear, upper, lower, left, right", "lateral, vertical, horizontal", and "top, bottom", etc., are generally based on the azimuth or positional relationships shown in the drawings, merely to facilitate description of the present application and simplify the description, and these azimuth terms do not indicate and imply that the apparatus or elements referred to must have a specific azimuth or be constructed and operated in a specific azimuth, and thus should not be construed as limiting the scope of protection of the present application; the orientation word "inner and outer" refers to inner and outer relative to the contour of the respective component itself.
Spatially relative terms, such as "above … …," "above … …," "upper surface at … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial location relative to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "above" or "over" other devices or structures would then be oriented "below" or "beneath" the other devices or structures. Thus, the exemplary term "above … …" may include both orientations of "above … …" and "below … …". The device may also be positioned in other different ways and the spatially relative descriptions used herein are construed accordingly.
In addition, the terms "first", "second", etc. are used to define the components, and are only for convenience of distinguishing the corresponding components, and the terms have no special meaning unless otherwise stated, and therefore should not be construed as limiting the scope of the present application.
Referring to fig. 1 to 3, the process of impurity doping in the crystal growth process of the czochralski method according to the present application will now be described.
The single crystal furnace in the process adopts the existing single crystal furnace with the auxiliary chamber, and comprises a main chamber and the auxiliary chamber, wherein a crucible is arranged in the main chamber, molten liquid is stored in the crucible, the auxiliary chamber is arranged on the upper side of the main chamber, and the on-off of the auxiliary chamber and the main chamber is controlled through a gate valve.
It is to be understood that when the single crystal furnace is used for seeding, the resistivity of the crystal is detected, and when the resistivity of the pulled crystal is not suitable, the resistivity of the crystal is regulated by an impurity complementary doping process in the crystal growth process of the Czochralski method; if the resistivity is qualified, continuing normal production.
Embodiment one:
the impurity complementary doping process in the crystal growth process of the Czochralski method comprises the following steps of:
a, as shown in FIG. 1, the shoulder 10 is discharged by cooling;
b, lifting at a speed of 4mm/S in 2 first preset stages, namely lifting 25cm firstly, cooling for 2 minutes, lifting 25cm again, lifting the total height of 50cm, and waiting for 5 minutes to enable the shoulder 10 to be fully cooled;
c, as shown in FIG. 2, the edge of the shoulder 10 is lowered below the liquid level of the molten metal at the speed of 8mm/S, the edge of the shoulder 10 is 1mm below the liquid level, the crucible is given a rotation speed of 1r/min, the crystal is rotated for 8r/min, the stability is 1min, the shoulder 10 is lifted out of the liquid level at the speed of 6mm/S, and a step-shaped groove 20 appears at the edge of the shoulder 10;
d, closing the crucible rotation and the crystal rotation, lifting the shoulder 10 at a speed of 6mm/S for 15cm, cooling for 2min as a second preset stage, lifting to the auxiliary chamber of the single crystal furnace in 4 second preset stages, closing the gate valve, and waiting for 10min to cool the shoulder 10;
e, opening the auxiliary chamber door, and placing 20mg of antimony dopant into the stepped groove 20 by using stainless steel tweezers;
f, after the furnace door is closed and pumped out, the gate valve is opened, the whole shoulder 10 is lowered to be below the liquid level of the melt at the speed of 7mm/S for melting and doping, and the resistivity of the crystals reaches the target value after doping.
The impurity complementary doping process in the crystal growth process of the Czochralski method provided by the embodiment of the application has the beneficial effects that: compared with the prior art, the impurity complementary doping process in the crystal growth process of the Czochralski method provided by the embodiment of the application is operated for 1.4 hours in the whole process, which is about 70 hours shorter than the drawing of restarting the furnace, 10.4 hours are saved compared with the complementary doping mode of repeatedly unloading a high-purity graphite device or punching seed crystals, and the complementary doping in the crystal pulling process of successful experiments is realized, so that the production cost is greatly saved and the production efficiency is improved; meanwhile, the process does not involve the introduction of an external device and the transformation of seed crystals, so that the risk of secondary impurity pollution is avoided greatly.
Embodiment two:
the impurity complementary doping process in the crystal growth process of the Czochralski method comprises the following steps of:
a, as shown in FIG. 1, remains the shoulder 10 after remelting by the crystal;
b, lifting the shoulder 10 at a speed of 6mm/S for 20cm, cooling for 3min to obtain a first preset stage, lifting the shoulder 10 at a total height of 60cm in 3 first preset stages, and waiting for 10min to sufficiently cool the shoulder 10;
c, as shown in FIG. 2, lowering the edge of the shoulder 10 below the liquid level of the molten metal at a speed of 6mm/S, keeping the edge of the shoulder 10 3mm below the liquid level, giving a crucible turn of 1.5r/min, a crystal turn of 10r/min, stabilizing for 3min, raising the shoulder 10 out of the liquid level at a speed of 4mm/S, and forming a stepped groove 20 at the edge of the shoulder 10;
d, closing the crucible rotation and the crystal rotation, lifting the shoulder 10 by 20cm at a speed of 4mm/S, cooling for 3min to be a second preset stage, lifting to the auxiliary chamber of the single crystal furnace in 3 second preset stages, closing the gate valve, and waiting for 15min to cool the shoulder 10;
e, opening the auxiliary chamber door and placing 15mg of antimony dopant into the stepped groove 20 using stainless steel tweezers;
f, after the furnace door is closed and pumped out, opening a gate valve, and lowering the whole shoulder 10 to be below the liquid level of the melt at the speed of 6mm/S to carry out melting and doping, wherein the resistivity of the crystals reaches the target value after doping.
The impurity complementary doping process in the crystal growth process of the Czochralski method provided by the embodiment of the application has the beneficial effects that: compared with the prior art, the impurity complementary doping process in the crystal growth process of the Czochralski method provided by the embodiment of the application is operated for 1.8 hours in the whole process, which is shortened by about 118 hours compared with the process of re-opening the furnace for drawing, 10.2 hours are saved compared with the complementary doping mode of repeatedly unloading the high-purity graphite device or seed crystal for punching, and the complementary doping is carried out in the process of successfully experimental crystal pulling, so that the production cost is greatly saved and the production efficiency is improved; meanwhile, the process does not involve the introduction of an external device and the transformation of seed crystals, so that the risk of secondary impurity pollution is avoided greatly.
In the above embodiments, the growth process of germanium crystal is taken as an example, and different crystals, such as silicon (Si), germanium (Ge), gallium arsenide (GaAs), gallium phosphide (GaP), indium phosphide (InP), ruby, white precious stone, yttrium aluminum garnet, spinel, etc., have different parameters, such as pulling speed, lifting height, cooling time, impurity type and weight, crucible rotation, crystal rotation, etc., involved in each step of the complementary doping process, so that those skilled in the art can obtain data through limited experiments according to the impurity complementary doping process in the crystal growth process of the czochralski method provided by the present application, and the data should be included in the protection scope of the present application.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.
Claims (6)
1. The impurity complementary doping process in the crystal growth process of the Czochralski method is characterized by comprising the following steps of:
a, discharging the shoulder (10) through cooling or reserving the shoulder (10) after crystal remelting;
lifting the shoulder (10) by a first preset height, waiting for a first preset time for cooling the shoulder (10);
c, lowering the crystal, enabling the edge of the shoulder (10) to be below the liquid level, giving crucible rotation, crystal rotation, stabilizing for a second preset time, then lifting the shoulder (10) out of the liquid level, observing whether a step-shaped groove (20) is formed in the shoulder (10), and repeating the step B, C if the step-shaped groove is not formed; if the step-like groove (20) is present, proceeding to the next step;
d, closing the crucible rotation and the crystal rotation, lifting the shoulder (10) into a secondary chamber of the single crystal furnace, closing a gate valve between a main chamber and the secondary chamber, and waiting for a third preset time to cool the shoulder (10);
e, opening the auxiliary chamber, and putting impurities to be doped into the step-shaped groove (20);
f, closing the auxiliary chamber, evacuating, opening the gate valve, and lowering the shoulder (10) below the liquid level to perform melting and doping.
2. The process for the impurity doping during the crystal growth by the Czochralski method as claimed in claim 1, wherein in the step A, the shoulder (10) is lifted at a speed of 4 to 6 mm/S.
3. The process of claim 2, wherein in step B, the shoulder (10) is lifted in two to three first predetermined stages, the total height of the lifted shoulder is the first predetermined height, the first predetermined height is 50 to 60cm, and the first predetermined time is 5 to 10min; wherein, the lifting is 20-30 cm, and the cooling is carried out for 1-3 min as a first preset stage.
4. The process of claim 1, wherein in step C, the edge of the shoulder (10) is lowered to 1-3 mm below the liquid level of the melt at a rate of 6-8 mm/S, the crucible is turned to 0.5-2 r/min, the crystal is turned to 5-10 r/min, and the second preset time is 1-3 min.
5. The process of claim 1, wherein in step D, the shoulder (10) is lifted into the sub-chamber in three to four second preset stages at a speed of 4 to 6mm/S, the third preset time being 10 to 15min; wherein, lifting by 15-20 cm, and cooling for 1-3 min is used as the second preset stage.
6. The process for the supplemental doping of impurities in the course of crystal growth by the czochralski method as claimed in claim 1, wherein in step F, the shoulder (10) is lowered below the liquid level at a speed of 6 to 8mm/S for melt supplemental doping.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012041200A (en) * | 2010-08-12 | 2012-03-01 | Nippon Telegr & Teleph Corp <Ntt> | Crystal growth method |
| CN105200513A (en) * | 2015-10-19 | 2015-12-30 | 天津市环欧半导体材料技术有限公司 | Novel Czochralski silicon single crystal doping method with resistivity control function |
| CN108796603A (en) * | 2018-08-29 | 2018-11-13 | 内蒙古中环协鑫光伏材料有限公司 | A kind of process of pulling of crystals doping up alloy |
| CN115613125A (en) * | 2022-11-07 | 2023-01-17 | 宁夏协鑫光伏科技有限公司 | Doping process of silicon material dopant |
| CN115821366A (en) * | 2022-12-09 | 2023-03-21 | 宁夏中欣晶圆半导体科技有限公司 | Boron and lightly-doped phosphorus supplementing method and crystal bar combined drawing and crystal orientation conversion drawing method |
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2023
- 2023-06-30 CN CN202310792282.2A patent/CN116815296A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012041200A (en) * | 2010-08-12 | 2012-03-01 | Nippon Telegr & Teleph Corp <Ntt> | Crystal growth method |
| CN105200513A (en) * | 2015-10-19 | 2015-12-30 | 天津市环欧半导体材料技术有限公司 | Novel Czochralski silicon single crystal doping method with resistivity control function |
| CN108796603A (en) * | 2018-08-29 | 2018-11-13 | 内蒙古中环协鑫光伏材料有限公司 | A kind of process of pulling of crystals doping up alloy |
| CN115613125A (en) * | 2022-11-07 | 2023-01-17 | 宁夏协鑫光伏科技有限公司 | Doping process of silicon material dopant |
| CN115821366A (en) * | 2022-12-09 | 2023-03-21 | 宁夏中欣晶圆半导体科技有限公司 | Boron and lightly-doped phosphorus supplementing method and crystal bar combined drawing and crystal orientation conversion drawing method |
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