CN117779179B - Single crystal growth device and single crystal growth method - Google Patents
Single crystal growth device and single crystal growth method Download PDFInfo
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- CN117779179B CN117779179B CN202410199685.0A CN202410199685A CN117779179B CN 117779179 B CN117779179 B CN 117779179B CN 202410199685 A CN202410199685 A CN 202410199685A CN 117779179 B CN117779179 B CN 117779179B
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- 239000013078 crystal Substances 0.000 title claims abstract description 82
- 238000002109 crystal growth method Methods 0.000 title claims abstract description 16
- 238000004321 preservation Methods 0.000 claims abstract description 14
- 230000001105 regulatory effect Effects 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 33
- 230000008569 process Effects 0.000 claims description 29
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 7
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000001154 acute effect Effects 0.000 claims description 4
- 230000007423 decrease Effects 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 6
- 230000033228 biological regulation Effects 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 54
- 230000002093 peripheral effect Effects 0.000 description 6
- 230000007246 mechanism Effects 0.000 description 5
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 238000005273 aeration Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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Abstract
The invention belongs to the technical field of single crystal growth equipment, and particularly relates to a single crystal growth device and a single crystal growth method, comprising the following steps: the air charging part is integrally arranged at the middle opening of the heat preservation cover and is provided with a first air flow channel, an upper air inlet, a side air outlet and a bottom air outlet which are respectively communicated with the first air flow channel; the mandrel is at least partially sleeved in the first airflow channel, a second airflow channel with a mandrel air inlet and a mandrel air outlet is formed in the mandrel, a protruding part is arranged outside a part of the mandrel between the mandrel air inlet and the mandrel air outlet, the mandrel and the inflatable part can relatively move in the airflow direction, and the airflow proportion flowing to the side air outlet and the second airflow channel through the first airflow channel is regulated through the protruding part. The invention can realize the temperature regulation and control of the upper end face of the crucible, ensure the temperature uniformity of the upper end face of the crucible, and improve the growth stability of single crystals, thereby being beneficial to the high-quality growth of single crystals.
Description
Technical Field
The invention belongs to the technical field of single crystal growth equipment, and particularly relates to a single crystal growth device and a single crystal growth method.
Background
Currently, the physical vapor transport method (PVT method) is a mainstream process technique for growing single crystals (e.g., silicon carbide single crystals), which is characterized in that a polycrystalline raw material is charged at the bottom of a crucible, a seed sheet (e.g., a silicon carbide seed wafer) is bonded to a graphite seed susceptor and is mounted at the upper portion of the crucible, and the single crystals are grown on the seed crystal by heating and sublimating the polycrystalline raw material at the bottom of the crucible.
During the single crystal growth process, process gases are introduced to regulate the pressure in the furnace and to establish a temperature gradient between the upper and lower end surfaces of the crucible. In the single crystal growth device in the prior art, process gas is directly filled into a working cavity of a hearth from an air charging port, a heat preservation cover, a crucible and a heater are arranged in the working cavity of the hearth, and the air charging port is positioned above the heat preservation cover.
However, the single crystal growth apparatus of the prior art is disadvantageous for stable growth of single crystals.
It should be noted that this section of the disclosure only provides a background related to the present disclosure, and does not necessarily constitute prior art or known technology.
Disclosure of Invention
The invention aims to overcome the defect that the growth stability of a single crystal growth device needs to be improved in the prior art, and provides the single crystal growth device and the single crystal growth method, which can realize the temperature regulation and control of the upper end face of a crucible, ensure the temperature uniformity of the upper end face of the crucible, improve the growth stability of single crystals and further facilitate the high-quality growth of the single crystals.
In order to achieve the above object, the present invention provides a single crystal growing apparatus comprising a crucible, a heater located at the outer side of the crucible, a heat-insulating cover provided outside the crucible and the heater, and a gas source; the middle part opening of heat preservation cover just opens and is located the top of crucible up end still includes:
The air charging part is integrally arranged at the middle opening of the heat preservation cover, the lower end of the air charging part extends along the direction close to the upper end face of the crucible and is provided with a first air flow channel, an upper air inlet, a side air outlet and a bottom air outlet, wherein the upper air inlet, the side air outlet and the bottom air outlet are respectively communicated with the first air flow channel, the upper air inlet is communicated with the air source, the bottom air outlet faces to the middle position of the upper end face of the crucible, and the side air outlet faces to the position close to the edge of the upper end face of the crucible;
The mandrel is at least partially sleeved in the first airflow channel, a second airflow channel with a mandrel air inlet and a mandrel air outlet is formed in the mandrel, the mandrel air inlet is communicated with the first airflow channel, the upper air inlet and the side air outlet, the mandrel air outlet is communicated with the bottom air outlet, a protruding portion is arranged outside a part of the mandrel between the mandrel air inlet and the mandrel air outlet, and the mandrel and the inflatable portion can move relatively in the airflow direction, so that the airflow proportion of the mandrel flowing to the side air outlet and the second airflow channel through the first airflow channel is adjusted through the protruding portion.
In some preferred embodiments of the invention, the side edges of the boss abut against the inner wall of the inflatable portion and are relatively movable in the direction of the air flow.
In some preferred embodiments of the present invention, the width of the convex portion is not smaller than the width of the side air outlet in the direction of the air flow.
In some preferred embodiments of the invention, the spindle air outlet is located at the side or middle of the bottom end of the spindle.
In some preferred embodiments of the present invention, the mandrel air outlet is located at a side of the mandrel, and a gap is left between a portion of the mandrel located below the protrusion and an inner wall of the inflatable portion, so that air at the mandrel air outlet flows out to the bottom air outlet.
In some preferred embodiments of the present invention, an inner wall of the inflatable portion near the bottom outlet forms an acute angle with the central axis of the inflatable portion.
In some preferred embodiments of the invention, the portion of the mandrel below the boss tapers in the direction of airflow, and the inner contour of the inflated portion near the bottom air outlet portion is identical to and conforms to the outer contour of the portion of the mandrel below the boss.
In some preferred embodiments of the invention, the mandrel air inlet is located at a side of the mandrel and in the direction of airflow, the mandrel air inlet is located between the upper air inlet and the side air outlet.
In some preferred embodiments of the invention, the upper air inlet is located at the top or upper side of the inflatable portion.
In some preferred embodiments of the present invention, the mandrel air inlet and the mandrel air outlet are both disposed at intervals or extended along the circumferential direction of the mandrel, and the side air outlets are disposed at intervals or extended along the circumferential direction of the inflatable portion.
In some preferred embodiments of the present invention, the air charging portion is fixedly installed at the opening in the middle of the heat insulation cover, and the top of the mandrel extends outwards along the air charging portion and is movably connected with the air charging portion, so that the mandrel can move relative to the air charging portion along the air flow direction.
In some preferred embodiments of the invention, the heater is higher than the upper end surface of the crucible.
In some preferred embodiments of the present invention, the upper portion of the heater is inclined in a direction approaching the upper end surface of the crucible.
In some preferred embodiments of the invention, the upper end or side of the crucible is curved.
In some embodiments of the invention, the single crystal is a silicon carbide single crystal or single crystal silicon.
The present invention also provides a single crystal growth method which grows in the single crystal growth apparatus, and which includes: in the single crystal growth process, the gas source is used for inflating the inflatable part, and the air is supplied to the upper end face of the crucible through the side air outlet and/or the bottom air outlet for controlling the temperature.
In some preferred embodiments of the present invention, the single crystal growth method further comprises: and the air supply temperature is controlled to different areas of the upper end surface of the crucible through the side air outlets and the bottom air outlets, the relative positions of the air charging part and the mandrel are regulated according to the required control Wen Qiliang of the different areas of the upper end surface of the crucible, and the air supply proportion of the process air from the air source from the side air outlets and the bottom air outlets of the air charging part is changed.
In some preferred embodiments of the present invention, the single crystal growth method further comprises: before single crystal growth, the single crystal is heated to a desired growth temperature by a heater.
Further preferably, in the initial stage of heating, when the temperature of the position, close to the edge, of the upper end face of the crucible is higher than the temperature of the position, close to the edge, of the middle of the upper end face of the crucible, air is supplied to the position, close to the edge, of the periphery of the upper end face of the crucible only through the side air outlets for controlling the temperature; along with the growth of single crystals, when the temperature of the position, close to the edge, of the upper end face of the crucible is lower than the temperature of the position, close to the edge, of the middle of the upper end face of the crucible, the relative positions of the inflating part and the mandrel are adjusted, and the air supply and temperature control are carried out on the position, close to the edge, of the middle and the periphery of the upper end face of the crucible through the air outlet at the bottom and the air outlet at the side face in different air proportions.
The beneficial effects are that:
The inventor of the invention finds that the position and the mode of filling process gas are key factors directly influencing the temperature and the temperature uniformity of the upper end face of the crucible, and the temperature uniformity of the upper end face of the crucible are one of key factors influencing the stable growth of single crystals, especially in the growth of large-size single crystals, the temperature difference of different areas of the upper end face of the crucible is larger, and the growth stability of the single crystals is greatly influenced. In the single crystal growth device in the prior art, process gas is filled from the outside of the heat preservation cover, then flows through the periphery of the heat preservation cover, does not pass through the upper end face of the crucible cover, cannot play a role in stabilizing and effectively regulating the temperature of the upper end face of the crucible, cannot effectively take away heat to form a high temperature gradient from top to bottom, and affects the stable growth of single crystals. Moreover, the process gases of the prior art cannot be efficiently utilized. Based on this, the present invention has been further studied.
According to the technical scheme, the inflating part and the mandrel with the specific structures are particularly arranged, so that process gas (namely, a gas source) can be respectively inflated to the middle part and the vicinity of the periphery of the upper end face of the crucible through the side gas outlet and the bottom gas outlet of the inflating part, on one hand, gas can be supplied through any one of the side gas outlet and the bottom gas outlet, or gas can be simultaneously supplied through the side gas outlet and the bottom gas outlet, selective accurate inflation and rapid temperature control can be carried out on a target area of the upper end face of the crucible, and the targeted stable and effective temperature regulation effect on the single crystal growth temperature distribution is achieved; on the other hand, the method can also be matched with the bulge, the opening and closing degree of the side air outlet and the mandrel air outlet can be changed by adjusting the relative movement of the mandrel in the air charging part, the flow direction of process gas and different air supply amounts to the periphery and the middle of the crucible are controlled, so that the process gas can charge and cool the middle and the periphery of the upper end face of the crucible controllably, the temperature of the upper end face of the crucible is regulated and controlled, the temperature of the upper end face of the crucible is ensured to be uniform, and the high-quality growth of single crystals is facilitated. The single crystal growth device can fully and efficiently utilize the process gas to control the temperature.
In addition, the side air outlets and the bottom air outlets of the invention have certain heights, and natural temperature difference exists when the side air outlets and the bottom air outlets are respectively inflated to the middle part and the peripheral two areas of the upper end face of the crucible, namely the temperature of the gas reaching the middle part of the upper end face of the crucible is higher, the temperature of the gas reaching the peripheral area of the upper end face of the crucible is lower, the temperature gradient of the upper end face of the crucible with the conditions of high middle temperature and low peripheral temperature after the crucible grows for a certain time can be reduced, the temperature uniformity of the upper end face of the crucible is facilitated, and the growth stability of single crystals is further improved.
The single crystal growth device has the advantages of simple structure, ingenious conception, easy implementation, stable performance, convenient operation and use and high repeatability, and can be widely applied to the growth of single crystals with various sizes, in particular to the growth of large-size single crystals.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural view showing an embodiment of a single crystal growing apparatus of the present invention.
Fig. 2 is a schematic view of the structure of the inflation part and the mandrel in fig. 1.
Description of the reference numerals
1.2 Parts of a crucible, 2 parts of a heater, 3 parts of a heat preservation cover, 4 parts of an inflation mechanism, 5 parts of a first airflow path, 6 parts of a second airflow path; 401. an inflation part; 402. a gap; 403. a mandrel air outlet; 404. a mandrel; 405. a side air outlet; 406. the mandrel air inlet; 407. upper air inlet 408, boss 409, first air flow channel 410, second air flow channel.
Detailed Description
In the description of the present invention, it should be understood that the terms "middle," "longitudinal," "transverse," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," etc. indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, are merely for convenience in describing the present invention and to simplify the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
The invention provides a single crystal growing device, as shown in figure 1, comprising a crucible 1, a heater 2 positioned on the outer side surface of the crucible 1, a heat preservation cover 3 arranged outside the crucible 1 and the heater 2, and an air source; the middle of the heat preservation cover 3 is opened, and the opening is positioned above the upper end face of the crucible 1.
In some embodiments, the heaters 2 are arranged in the outer circumferential direction of the crucible 1.
The gas source is process gas, and a person skilled in the art can select specific types according to actual requirements, so long as the purposes of required temperature and pressure adjustment and the like can be achieved.
As shown in fig. 2, the single crystal growth apparatus of the present invention further includes: the air charging part 401 is integrally arranged at the middle opening of the heat insulation cover 3, the lower end of the air charging part extends along the direction close to the upper end face of the crucible 1, and is provided with a first air flow channel 409, an upper air inlet 407, a side air outlet 405 and a bottom air outlet which are respectively communicated with the first air flow channel 409, the upper air inlet 407 is communicated with the air source, the bottom air outlet is oriented to the middle position of the upper end face of the crucible 1, and the side air outlet 405 is oriented to the position close to the edge of the upper end face of the crucible 1.
As shown in fig. 2, the single crystal growth apparatus of the present invention further includes: the mandrel 404 is at least partially sleeved in the first airflow channel 409, and a second airflow channel 410 with a mandrel air inlet 406 and a mandrel air outlet 403 is formed in the mandrel 404, the mandrel air inlet 406 is mutually communicated with the first airflow channel 409, the upper air inlet 407 and the side air outlet 405, the mandrel air outlet 403 is communicated with the bottom air outlet, a protruding portion 408 is arranged outside a part of the mandrel 404 between the mandrel air inlet 406 and the mandrel air outlet 403, and the mandrel 404 and the inflatable portion 401 can relatively move along the airflow direction so as to adjust the airflow proportion flowing to the side air outlet 405 and the second airflow channel 410 through the first airflow channel 409 through the protruding portion 408.
The inflating part 401 and the mandrel 404 form an inflating mechanism 4 for introducing an air source into the upper end face of the crucible 1, and the inflating mechanism 4 is arranged at the opening of the middle part of the heat preservation cover 3 in fig. 1. The inflation portion 401 and the mandrel 404 may be regular or irregular shafts, respectively.
In some preferred embodiments of the present invention, the side edges of the boss 408 abut against the inner wall of the air charging portion 401 and are relatively movable in the air flow direction. The side edges of the protruding portion 408 abut against the inner wall of the air charging portion 401, which means that they can contact with each other, so as to better control the opening and closing degree of the side air outlet 405 of the air charging portion 401.
In some preferred embodiments of the present invention, the width of the protrusion 408 is not smaller than the width of the side air outlet 405 in the air flow direction, which can form a seal or a partial opening to the side air outlet 405, thereby facilitating control of the air supply amount of the side air outlet 405.
In other embodiments, the side edges of the raised portion 408 are spaced from the inner wall of the plenum 401 or the raised portion 408 has a width less than the width of the side air outlet 405, in which case the side air outlet 405 may be controlled but limited in amount.
In some preferred embodiments of the present invention, the mandrel air outlet 403 is located at the side or middle of the bottom end of the mandrel 404. When the mandrel air outlet 403 is located in the middle of the bottom end of the mandrel 404, the portion of the second air flow channel 410 near the mandrel air outlet 403 may be distributed in a regular size (such as a column shape, a cone shape, etc.) or an irregular size (such as an S-shaped curve), and a blocking cover may or may not be further disposed at the mandrel air outlet 403.
In some more preferred embodiments of the invention, the mandrel air outlet 403 is located on the side of the mandrel 404, which can control the air flow direction or air flow stability through the gap 402 between the inner wall of the inflatable portion 401 and the mandrel 404.
Further, a gap 402 is left between the portion of the mandrel 404 located below the protruding portion 408 and the inner wall of the inflating portion 401, so that the gas at the gas outlet 403 of the mandrel flows out to the bottom gas outlet. In this preferred embodiment, the position of the mandrel 404 in the inflating portion 401 is adjusted to control the flow direction of the process gas, for example, when the boss 408 of the mandrel 404 moves up to seal the side gas outlet 405, the process gas flows out from the bottom gas outlet, or when the boss 408 moves down to the mandrel gas outlet 403 to seal the inner wall of the inflating portion 401, as shown in fig. 2, the process gas flows out from the side gas outlet 405, so that the process gas performs controllable inflation cooling on the center and the periphery of the upper end surface of the crucible 1.
In some preferred embodiments of the present invention, an inner wall of the air charging portion 401 near the bottom air outlet forms an acute angle with the central axis of the air charging portion 401. In this preferred solution, the inner wall of the air charging portion 401 near the bottom air outlet is a coanda curved surface, which is more beneficial for the airflow to flow out in coanda effect along the inner wall of the air charging portion 401 near the bottom air outlet, so as to further improve the stability of the airflow flowing out.
The specific angle of the acute angle can be determined according to the diameter of the crucible and the airflow direction range of the bottom air outlet, and the temperature of the middle high-temperature area of the upper end surface of the crucible can be reduced conveniently.
In some preferred embodiments of the present invention, the upper end or side of the crucible 1 is curved in coanda so that the gas flow stably flows along the upper surface thereof.
In some preferred embodiments of the present invention, the portion of the mandrel 404 below the boss 408 gradually decreases in transverse diameter in the direction of airflow, and the inner contour shape of the air-filled portion 401 near the bottom air outlet is identical to and matches the outer contour shape of the portion of the mandrel 404 below the boss 408. In the preferred scheme, the lower parts of the inflating part 401 and the mandrel 404 are preferably in conical surface fit, so that the opening and closing degree of the side air outlet 405 and the mandrel air outlet 403 can be adjusted more quickly, and the air flow stability is improved.
The cross-diameter of the portion of the mandrel 404 below the boss 408 is gradually reduced, which may be a continuous reduction in cross-diameter, or a stepwise gradient of cross-diameters (e.g., a cross-diameter of a first height in the vertical direction is greater than a cross-diameter of a second height below), preferably the former. The bottom of the mandrel 404 is preferably planar.
The inner contour shape of the air-charging portion 401 near the bottom air outlet is identical to and matches with the outer contour shape of the portion of the mandrel 404 located below the protruding portion 408, which means that, when the lower end surface of the mandrel 404 is flush with the lower end surface of the air-charging portion 401, the inner contour shape of the air-charging portion 401 near the bottom air outlet completely matches with the outer contour shape of the portion of the mandrel 404 located below the protruding portion 408, so as to form a seal.
The mandrel air inlet 406 may be located on the side or top of the mandrel 404 where the mandrel 404 may be secured to a drive structure by a connecting rod. In some preferred embodiments of the present invention, the mandrel inlet 406 is located on the side of the mandrel 404 and in the direction of the gas flow, the mandrel inlet 406 is located between the upper inlet 407 and the side outlet 405, which further facilitates the redistribution of process gas from the first gas flow channel 409 into the side outlet 405 and the second gas flow channel 410.
In some preferred embodiments of the invention, the upper air inlet 407 is located at the top or upper side of the plenum 401. When the upper air inlets 407 are located on the upper side of the air charging portion 401, a plurality of upper air inlets 407 are preferably arranged at intervals in the circumferential direction of the air charging portion 401, which is more beneficial to stabilizing the air flow.
In some preferred embodiments of the present invention, the mandrel air inlet 406 and the mandrel air outlet 403 are both disposed at intervals or extended along the circumferential direction of the mandrel 404, and the side air outlet 405 is disposed at intervals or extended along the circumferential direction of the inflatable portion 401. Wherein, the arrangement is preferable, and at this time, the corresponding ports may be respectively arranged in at least three of the circumferential directions. When extending the setting, mean that corresponding mouth is the opening that extends along circumferencial direction in succession, and the fixed of upper and lower pipe can be fixed through the connecting rod this moment, and the connecting rod can set up at the middle part or the outside of corresponding axle.
In the present invention, the mode of the mandrel 404 and the inflatable portion 401 that can relatively move in the air flow direction may have a wide selectable range, specifically, the inflatable portion 401 may be fixed, the mandrel 404 may be moved, the inflatable portion 401 may be fixed, or the mandrel 404 and the inflatable portion 401 may simultaneously move but have different moving speeds, so long as the mandrel 404 and the inflatable portion 401 can relatively move in the air flow direction.
In some preferred embodiments of the present invention, the air-filling portion 401 is fixedly installed at the opening in the middle of the heat-preserving cover 3, and the top of the mandrel 404 extends outwards along the air-filling portion 401 and is movably connected with the air-filling portion 401, so that the mandrel 404 can move relative to the air-filling portion 401 along the air flow direction. In the preferred scheme, the heights of the side air outlets 405 and the bottom air outlets are more convenient to fix, the air supply flow is accurately regulated, and the temperature is accurately and quantitatively controlled for the growth of single crystals with specific sizes.
The movable connection between the mandrel 404 and the inflatable portion 401 is a slidable seal, for example, the movable connection may be a graphite felt seal ring seal, a small gap seal, or the like.
The moving driving mechanism may be any device capable of driving the mandrel 404 to move in the prior art, and will not be described herein.
In some preferred embodiments of the present invention, the height of the heater 2 is higher than the height of the upper end surface of the crucible 1, which can make the process gas more turn from the upper end surface of the crucible 1 to move along the side surface of the crucible 1, and can further cool the side surface of the crucible 1, especially cool the side surface of the crucible cover by aeration.
In some preferred embodiments of the present invention, the upper portion of the heater 2 is inclined toward the upper end face of the crucible 1, which is more beneficial for the process gas to rapidly and largely turn to move along the side face of the crucible 1, and can further cool the side face of the crucible 1.
It will be appreciated that the crucible 1 of the present invention comprises a crucible 1 body and a crucible cover. The crucible 1 body is used for loading polysilicon raw materials, and the middle part of the inner part of the crucible cover can be used for installing seed crystals.
The single crystal growth apparatus of the present invention may further include conventional components such as a seed holder (preferably, a graphite seed holder) for bonding seed sheets, which are all conventional techniques as long as single crystal growth can be achieved, and will not be described herein.
In the growth device of different single crystals, the temperature distribution condition of the upper end face of the crucible is different in the single crystal growth process, for example, the upper end face of the crucible has the phenomena of high middle temperature and low peripheral temperature in the growth device of silicon carbide single crystals; for other single crystals such as single crystal silicon, the peripheral temperature of the upper end face of the crucible is high, the center temperature is low, the raised middle of the grown single crystal silicon crystal is serious, and the effective thickness of the effective single crystal is small. The single crystal growth device of the invention can be suitable for the growth of single crystals with different crucible temperature distribution, and the temperature can be controlled in a targeted manner by adjusting the air supply proportion of the side air outlet 405 and the bottom air outlet, thereby being beneficial to the high-quality growth of single crystals, for example, being suitable for the growth of silicon carbide single crystals or single crystal silicon, and being particularly suitable for the growth of silicon carbide single crystals.
The single crystal growth device of the invention can adopt at least three air supply modes: firstly, only the bottom air outlet of the air charging part 401 is started, at this time, only the mandrel 404 is required to be moved to a position, so that the bulge 408 blocks the side air outlet 405, and the process air of the air source flows out sequentially through the upper air inlet 407, the first air flow channel 409, the second air flow channel 410, the mandrel air outlet 403 and the bottom air charging port, and is supplied to the middle area of the upper end surface of the crucible 1; secondly, only the side air outlet 405 of the air charging part 401 is started, at this time, the protruding part 408 is located below the side air outlet 405, the bottom air outlet is sealed by the inner wall of the air charging part 401 (at this time, the mandrel air outlet 403 is located at the side of the mandrel 404) or an additionally arranged blocking cover (at this time, the mandrel air outlet 403 is located at the middle part of the bottom end of the mandrel 404), and the process air of the air source flows out sequentially through the upper air inlet 407, the first air flow channel 409 and the side air outlet 405, and is supplied towards the peripheral area of the upper end surface of the crucible 1; thirdly, the bottom air outlet and the side air outlet 405 of the air charging part 401 supply air at the same time, at this time, the mandrel 404 moves upwards, as shown in fig. 2, a gap 402 is reserved between the head of the mandrel 404 and the inner wall of the air charging part 401, the air source enters from the upper air inlet 407 of the air charging part 401 and flows through the first air flow channel 409, one part supplies air to the periphery of the upper end face of the crucible 1 through the side air outlet 405, and the other part supplies air to the middle area of the upper end face of the crucible 1 through the second air flow channel 410, the mandrel air inlet 406 and the mandrel air outlet 403; the upper and lower relative positions of the mandrel 404 and the air charging part 401 (such as the part of the bulge part 408 which plugs the side air outlet 405, and the opening size of the side air outlet 405 is reduced) can be adjusted during the process, so that the air supply amount of the air source to the periphery and the middle of the upper end surface of the crucible 1 is changed, the temperature regulation and control of the upper end surface of the crucible 1 are realized, the temperature uniformity is ensured, and the stability of high-quality growth of single crystals is improved.
The present invention also provides a single crystal growth method which grows in the single crystal growth apparatus, and which includes: during the growth of the single crystal, the gas is filled into the gas filling part 401 by a gas source, and the gas is supplied to the upper end face of the crucible 1 through the side gas outlet 405 and/or the bottom gas outlet for controlling the temperature.
In some preferred embodiments of the present invention, the single crystal growth method further comprises: the air supply and temperature control are carried out to different areas of the upper end face of the crucible 1 through the side air outlets 405 and the bottom air outlets, the relative positions of the air charging part 401 and the mandrel 404 are regulated according to the required control Wen Qiliang of the different areas of the upper end face of the crucible 1, and the air supply proportion of the process air from the air source from the side air outlets 405 and the bottom air outlets of the air charging part 401 is changed.
In some preferred embodiments of the present invention, the single crystal growth method further comprises: before the single crystal growth, it is heated to a desired growth temperature by the heater 2.
Further preferably, in the initial stage of heating, when the temperature of the upper end face of the crucible 1 near the edge is higher than the temperature of the middle position of the upper end face of the crucible 1, air is supplied to the periphery of the upper end face of the crucible 1 near the edge only through the side air outlets for controlling the temperature; along with the growth of single crystals, when the temperature of the upper end face of the crucible 1 near the edge is lower than the temperature of the middle position of the upper end face of the crucible 1, the relative positions of the inflating part 401 and the mandrel 404 are adjusted, and the air supply and temperature control are carried out on the middle position and the periphery near the edge of the upper end face of the crucible 1 through the bottom air outlet matched with the side air outlet 405 in different air proportions.
In the present invention, in the initial stage, the heater 2 heats the periphery of the crucible cover by heat radiation and heat convection, the temperature of the periphery of the crucible cover is high, and the temperature of the middle part is low, and at this time, the process gas flows out from the side gas outlet 405, flows along the first gas flow path 5 as shown in fig. 1, and carries part of the heat energy, thereby reducing the temperature difference between the periphery and the middle part of the crucible cover.
With the increase of the heating time and the continuous growth of the single crystal, the temperature in the middle of the crucible cover is continuously increased, and at this time, if the gas is still discharged according to the side gas outlet 405, more heat energy around the crucible cover is taken away, so that the temperature around the crucible cover is lower than the temperature in the middle of the crucible cover, which is unfavorable for the stable growth of the single crystal. In contrast, by adjusting the air charging mechanism 4, as shown in fig. 1, a part of process gas flows through the second airflow channel 410 and flows out of the mandrel air outlet 403, and the heat energy in the middle of the crucible cover is taken away by the second airflow path 6, so that the temperature unevenness of the crucible cover is reduced; and the position of the mandrel 404 is adjusted to ensure that the air outlet ratio of the side air outlet 405 and the mandrel air outlet 403 is proper, so that the uniformity of temperature at different position areas of the crucible cover can be realized, and the stable and high-quality growth of single crystals can be realized.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (13)
1. A single crystal growing device comprises a crucible, a heater positioned on the outer side surface of the crucible, a heat preservation cover arranged outside the crucible and the heater, and an air source; the middle part opening of heat preservation cover just opens and is located the top of crucible up end, its characterized in that still includes:
The air charging part is integrally arranged at the middle opening of the heat preservation cover, the lower end of the air charging part extends along the direction close to the upper end face of the crucible and is provided with a first air flow channel, an upper air inlet, a side air outlet and a bottom air outlet, wherein the upper air inlet, the side air outlet and the bottom air outlet are respectively communicated with the first air flow channel, the upper air inlet is communicated with the air source, the bottom air outlet faces to the middle position of the upper end face of the crucible, and the side air outlet faces to the position close to the edge of the upper end face of the crucible;
The mandrel is at least partially sleeved in the first airflow channel, a second airflow channel with a mandrel air inlet and a mandrel air outlet is formed in the mandrel, the mandrel air inlet is communicated with the first airflow channel, the upper air inlet and the side air outlet, the mandrel air outlet is communicated with the bottom air outlet, a protruding portion is arranged outside a part of the mandrel between the mandrel air inlet and the mandrel air outlet, the mandrel and the inflatable portion can move relatively in the airflow direction, so that the airflow proportion of the first airflow channel flowing to the side air outlet and the second airflow channel is regulated through the protruding portion, the side edge of the protruding portion abuts against the inner wall of the inflatable portion and can move relatively in the airflow direction, and the width of the protruding portion in the airflow direction is not smaller than the width of the side air outlet, and the mandrel air inlet is located on the side face of the mandrel and between the upper air inlet and the side air outlet in the airflow direction.
2. The single crystal growing apparatus of claim 1 wherein the mandrel air outlet is located at a side or bottom middle of the mandrel.
3. The single crystal growing apparatus according to claim 2, wherein the mandrel gas outlet is located at a side of the mandrel, and a gap is left between a portion of the mandrel located below the boss and an inner wall of the gas charging portion, so that gas at the mandrel gas outlet flows out to the bottom gas outlet.
4. The single crystal growing apparatus of claim 3, wherein an inner wall of the gas charging portion near the bottom gas outlet forms an acute angle with the central axis of the gas charging portion.
5. The single crystal growing apparatus according to claim 4, wherein a portion of the mandrel located below the boss portion gradually decreases in transverse diameter in a direction of the gas flow, and an inner contour shape of the gas-filled portion near the bottom gas outlet portion is identical to and conforms to an outer contour shape of the portion of the mandrel located below the boss portion.
6. The single crystal growing apparatus according to any one of claims 1 to 5, wherein the upper air inlet is located at a top or upper side of the air charging portion; the mandrel air inlets and the mandrel air outlets are arranged or extend along the circumferential direction of the mandrel at intervals, and the side air outlets are arranged or extend along the circumferential direction of the inflatable part at intervals.
7. The single crystal growing apparatus according to any one of claims 1 to 5, wherein a height of the heater is higher than a height of an upper end face of the crucible; and/or the upper part of the heater is obliquely arranged in a direction approaching to the upper end face of the crucible.
8. The apparatus according to any one of claims 1 to 5, wherein an upper end surface or a side surface of the crucible is a coanda curved surface.
9. The apparatus according to any one of claims 1 to 5, wherein the air charging portion is fixedly installed at a central opening of the heat-insulating cover, and a top portion of the mandrel extends outward along the air charging portion and is movably connected to the air charging portion so as to allow the mandrel to move relative to the air charging portion in a direction of air flow.
10. The single crystal growth apparatus according to any one of claims 1 to 5, wherein the single crystal is a silicon carbide single crystal.
11. A single crystal growth method, characterized in that it grows in the single crystal growth apparatus according to any one of claims 1 to 10, and that it comprises: in the single crystal growth process, the gas source is used for inflating the inflatable part, and the air is supplied to the upper end face of the crucible through the side air outlet and/or the bottom air outlet for controlling the temperature.
12. The single crystal growth method according to claim 11, wherein the single crystal growth method further comprises: and the air supply temperature is controlled to different areas of the upper end surface of the crucible through the side air outlets and the bottom air outlets, the relative positions of the air charging part and the mandrel are regulated according to the required control Wen Qiliang of the different areas of the upper end surface of the crucible, and the air supply proportion of the process air from the air source from the side air outlets and the bottom air outlets of the air charging part is changed.
13. The single crystal growth method according to claim 11, wherein the single crystal growth method further comprises: heating to a desired growth temperature by a heater prior to single crystal growth; in the initial heating stage, when the temperature of the position, close to the edge, of the upper end face of the crucible is higher than the temperature of the position, close to the edge, of the middle of the upper end face of the crucible, air is supplied to the position, close to the edge, of the periphery of the upper end face of the crucible through the side air outlets only for controlling the temperature; along with the growth of single crystals, when the temperature of the position, close to the edge, of the upper end face of the crucible is lower than the temperature of the position, close to the edge, of the middle of the upper end face of the crucible, the relative positions of the inflating part and the mandrel are adjusted, and the air supply and temperature control are carried out on the position, close to the edge, of the middle and the periphery of the upper end face of the crucible through the air outlet at the bottom and the air outlet at the side face in different air proportions.
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