Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a single crystal growing furnace which can solve the problems of uneven crystal growth and uneven oxygen content in a crystal bar.
The invention also provides a crystal growth method.
A single crystal growth furnace according to a first aspect of the present invention comprises: the furnace body is internally provided with a furnace chamber; the crucible is arranged in the furnace chamber and used for containing molten liquid; the heater is arranged in the furnace chamber and surrounds the radial outer side of the crucible; insulation construction includes: the heat insulation device comprises a heat insulation part and an adjusting part, wherein the heat reflection coefficient or the heat absorption coefficient of the adjusting part is different from that of the heat insulation part, the adjusting part is arranged between the heat insulation part and the heater and can rotate relative to the heat insulation part, and the adjusting part is used for adjusting the area of the opposite surface of the heat insulation part and the heater.
According to the single crystal growth furnace, the heat preservation part with different heat reflection coefficients or heat preservation coefficients and the heat preservation structure of the adjusting part are arranged, the adjusting part can rotate relative to the heat preservation part, so that the relative area of the heat preservation part and the heater is changed, the heat transferred to the crucible by the heater is favorably controlled in the circumferential direction of the crucible, the fine adjustment of the heat of molten liquid in the crucible is realized, the uneven temperature distribution in the circumferential direction of the molten liquid is improved, and the problems of uneven crystal growth and uneven oxygen content in a crystal bar are solved.
In some embodiments, the thermal insulating member comprises: the reflecting part and the absorbing part are alternately connected, the heat reflectivity of the reflecting part is higher than that of the absorbing part, and the heat absorptivity of the absorbing part is higher than that of the reflecting part; the adjusting member includes: the reflection part or the absorption part.
In some embodiments, the heat insulating member is formed with first and second zones alternately arranged circumferentially along the heat insulating structure, one of the first and second zones being the reflecting portion, and the other of the first and second zones being the absorbing portion; the adjusting piece is formed with along the third district and the fourth district that insulation construction circumference set up in turn, the third district is reflection portion or absorption portion, the fourth district is hollow out construction.
In some embodiments, the thermal insulating member is rotatable relative to the regulating member between a first position and a second position, the fourth zone and the first zone at least partially coinciding when the regulating member is in the first position relative to the thermal insulating member; when the adjusting piece is in the second position relative to the heat preservation piece, the fourth area and the second area are at least partially overlapped.
In some embodiments, the insulation structure comprises: the side heat-insulating structure is sleeved on the radial outer side of the heater.
In some embodiments, the insulation structure comprises: and the bottom heat insulation structure is arranged in the furnace chamber and is positioned below the crucible.
In some embodiments, the reflective portion is formed of molybdenum and the absorptive portion is formed of graphite.
In some embodiments, the thermal insulating member and the regulating member each include: the furnace chamber comprises a first connecting part and a second connecting part which are arranged at intervals along the axial direction of the furnace chamber, and a plurality of main body parts which are arranged between the first connecting part and the second connecting part, wherein the first connecting part and the second connecting part are annular, and the main body parts are arranged along the circumferential direction of the first connecting part and the second connecting part.
In some embodiments, the single crystal growth furnace further comprises: and the driving mechanism is connected with the heat preservation piece and/or the adjusting piece and drives the heat preservation piece and the adjusting piece to rotate relatively.
According to the crystal growing method of the single crystal growing furnace of the second aspect of the present invention, a crystal is grown using the single crystal growing furnace according to the first aspect of the present invention, the crystal growing method comprising: and controlling the adjusting piece to rotate relative to the heat preservation piece, and adjusting the area of the opposite surface of the heat preservation piece and the heater, thereby adjusting the temperature in the furnace chamber.
According to the crystal growth method of the single crystal growth furnace, the stability of a solid-liquid interface is improved and the problem of impurity segregation is avoided by growing the crystal by using the single crystal growth furnace according to the embodiment of the first aspect of the invention, and the problems of uneven temperature distribution in the circumferential direction of the molten steel and uneven oxygen content in the crystal bar are solved by adjusting the thermal field in the direction parallel to the magnetic field.
Further, the single crystal growth furnace includes: a transverse magnetic field applying device arranged in the furnace chamber and used for applying a transverse magnetic field to the molten soup in the crucible,
the crystal growth method further includes: and controlling the relative position of the heat-insulating structure and the transverse magnetic field according to the direction of the transverse magnetic field, so that the heat reflection coefficient of the heat-insulating structure in the direction parallel to the transverse magnetic field is smaller than the heat reflection coefficient in the direction perpendicular to the transverse magnetic field.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are illustrative and intended to explain the present invention and should not be construed as limiting the present invention.
A single crystal growth furnace 100 according to an embodiment of the present invention is described below with reference to fig. 1 to 12.
As shown in fig. 1, a single crystal growth furnace 100 according to an embodiment of the present invention includes: the furnace comprises a furnace body 1, a crucible 2, a heater 3 and a heat preservation structure 4.
Specifically, be formed with stove room 11 in the furnace body 1, crucible 2 is arranged in the stove room 11 and is used for holding the molten steel, and heater 3 is arranged in the stove room 11 and encircles the radial outside of crucible 2, and insulation construction 4 includes: a heat insulating member 41 and an adjusting member 42. The adjusting member 42 is provided between the heat retaining member 41 and the heater 3, and is rotatable relative to the heat retaining member 41. The adjusting member 42 has a heat reflection coefficient or a heat absorption coefficient different from that of the heat retaining member 41 for adjusting the area of the facing surface of the heat retaining member 41 and the heater 3.
As described above, in the field of heat radiation, heat is projected to the surface of an object, and heat reflection, heat absorption, and heat transmission phenomena may occur. The thermal reflectivity is the ratio of the energy reflected by the surface of the object to the total energy projected to the object in the heat rays transmitted to the object, and the object with high thermal reflectivity reflects relatively more heat. The heat absorption rate is a ratio of absorbed energy to total energy projected in the heat ray projected onto the object, and the object having a high heat absorption rate absorbs relatively much heat. The heat transmission rate refers to the ratio of the energy transmitted in the heat rays projected on the surface of the object to the total energy projected on the surface, the heat loss of the object with high heat transmission rate is more, and the heat preservation performance is poorer than that of the former two.
The heat insulating member 41 and the adjusting member 42 disclosed in the embodiment of the present invention may be made of materials with low heat transmission rate and different heat reflection rate or heat absorption rate, so as to ensure the heat insulating performance of the heat insulating structure 4. The adjusting part 42 can rotate relative to the heat preservation part 41, and can shield the heat preservation part 41 between the heater 3 and the heat preservation part 41, thereby changing the heat preservation performance of the whole heat preservation structure 4 on the single crystal growth furnace 100 and further regulating and controlling the temperature of the furnace chamber 11.
In some embodiments of the present invention, the heat retaining member 41 has a reflection portion and an absorption portion alternately connected, the reflection portion having a higher thermal reflectance than the absorption portion, and the absorption portion having a higher thermal absorptivity than the reflection portion. The adjusting member 42 includes: a reflective portion or an absorptive portion.
The reflecting portion reflects a part of the heat ray into the furnace chamber 11 upon receiving the heat generated by the heater, the absorbing portion absorbs a part of the heat ray upon receiving the heat generated by the heater 3, the amount of heat reflected by the reflecting portion is larger than the amount of heat reflected by the absorbing portion, and the amount of heat absorbed by the absorbing portion is larger than the amount of heat absorbed by the reflecting portion. In the embodiment of the invention, the heat preservation piece 41 is arranged between the furnace body 1 and the heater 3, the heat preservation piece 41 and the heater 3 have opposite surfaces, the heat reflectivity of the reflection part in the heat preservation piece 41 is higher than that of the absorption part, the heat absorptivity of the absorption part is higher than that of the reflection part, the areas of the reflection part and the absorption part at the parts opposite to the heater 3 are adjustable, and whether the area of the reflection part is larger or the area of the absorption part is larger in the opposite surfaces of the heat preservation piece 41 and the heater 3 can be controlled, so that the heat preservation piece 41 disclosed by the embodiment of the invention can adjust the reflected heat and the absorbed heat, and further can finely adjust the temperature in the furnace chamber 11. In addition, it should be noted that, in the actual crystal growth process, the crucible 2 needs to rotate continuously, so that although the heat insulating member 41 of the embodiment of the present invention has two different materials, the relative rotation of the heat insulating member 41 and the crucible 2 can equalize the temperature difference in the circumferential direction of the crucible 2, and stabilize the thermal field. The reflecting portion and the absorbing portion may have the same or different relative areas to the crucible 2, and the areas of the reflecting portions may be the same or different. The reflective portions and the absorptive portions of the heat retaining member 41 may be alternately arranged at intervals, or the reflective portions may be continuously arranged or the absorptive portions may be continuously arranged.
In some embodiments of the present invention, as shown in fig. 2, the insulating member 41 is formed with first and second sections 4121 and 4122 alternately arranged circumferentially along the insulating structure 4, one of the first and second sections 4121 and 4122 being a reflecting portion, and the other of the first and second sections 4121 and 4122 being an absorbing portion; the adjusting member 42 is formed with a third region 4111 and a fourth region 4112 which are alternately arranged along the circumference of the heat insulation structure 4, the third region 4111 is a reflection portion or an absorption portion, and the fourth region 4112 is a hollow structure.
The fourth area of the adjusting member 412 is a hollow area, and the area of the reflecting portion or the absorbing portion of the heat insulating member 41 facing the heater 3 can be controlled by the relative rotation of the adjusting member 42 and the heat insulating member 41. When the area of the reflection portion facing the heater 3 is large, the total amount of heat received by the heater 3 is high, and when the area of the absorption portion received by the heater 3 is large, the total amount of heat received by the heater 3 is low.
In some embodiments of the present invention, the thermal insulating member 41 is rotatable relative to the adjusting member 42 between a first position and a second position, and when the adjusting member 42 is in the first position relative to the thermal insulating member 41, the fourth region 4112 and the first region 4121 at least partially coincide; when the adjusting member 42 is in the second position relative to the insulating member 41, the fourth region 4112 and the second region 4122 are at least partially coincident.
Illustratively, as shown in fig. 3 and 4, the heat retaining member 41 includes a reflection portion and an absorption portion, and the adjusting member 42 includes a reflection portion and a hollow structure, and the hollow structure is opposite to the reflection portion of the heat retaining member 41, so that the heat retaining member 41 opposite to the heater 3 is the reflection portion, and at this time, the heat of the furnace chamber 11 is the highest under the condition that the heating power of the heater 3 is not changed. As shown in fig. 5, the adjusting member 42 and the heat retaining member 41 are adjusted to rotate relatively, so that the hollowed-out structure corresponds to the adjacent reflection portion and absorption portion of the heat retaining member 41, and since the adjusting member 42 is a reflection portion, the area of the reflection portion of the heat retaining member 41 opposite to the heater 3 is larger than that of the absorption portion, and at this time, the amount of heat received by the crucible 2 is high under the condition that the heating power of the heater 3 is not changed. As shown in fig. 6 and 7, the heat insulating member 41 includes a reflection portion and an absorption portion, the adjusting member 42 includes an absorption portion and a hollow structure, the hollow structure corresponds to the reflection portion of the heat insulating member 41, the heat insulating member 41 has both the reflection portion and the absorption portion opposite to the crucible 2, and the temperature in the furnace chamber 11 is lower than the two. As shown in fig. 8 and 9, the hollow structure corresponds to the absorption portion of the heat insulating material 41, and only the absorption portion of the heat insulating material 41 facing the crucible 2 is provided, and the temperature of the furnace chamber 11 is the lowest as described above. As shown in fig. 10, the hollow structure corresponds to the reflection portion and the absorption portion adjacent to the heat retaining material 41, and in this case, the area of the heat retaining material 41 and the heater 3 with respect to the absorption portion is larger than the area of the reflection portion.
In some embodiments of the present invention, as shown in fig. 11, the insulation structure 4 comprises: the side heat-insulating structure 41 is sleeved on the radial outer side of the heating device 3, the side heat-insulating structure 41 is provided with an inner heat-insulating layer 411 and an outer heat-insulating layer 412, the heat-insulating part 41 is formed into the outer heat-insulating layer 412, and the adjusting part 42 is formed into the inner heat-insulating layer 411. Accordingly, the side heat insulating structure 41 has a simple overall structure, the inner heat insulating layer 411 and the outer heat insulating layer 412 can rotate relatively, the area ratio of the reflection portion and the absorption portion is changed, and the temperature of the furnace chamber 11 is finely adjusted in the direction radially outward of the heater 3.
In some embodiments of the invention, as shown in fig. 12, the insulation structure 4 comprises: the bottom heat preservation structure 42 is arranged in the furnace chamber 11 and located below the crucible 2, the bottom heat preservation structure 42 is provided with an upper heat preservation layer 421 and a lower heat preservation layer 422, the heat preservation part 41 is formed into the lower heat preservation layer 422, and the adjusting part 42 is formed into the upper heat preservation layer 421. Accordingly, the bottom heat insulating structure 42 has a simple overall structure, and the upper heat insulating layer 421 and the lower heat insulating layer 422 rotate relative to each other, thereby changing the area ratio of the reflection portion and the absorption portion and finely adjusting the temperature of the oven chamber 11 from below the heater 3.
Because molybdenum has a large heat reflectivity and a small heat absorptivity, graphite has a large heat absorptivity and a small heat reflectivity, the reflecting part is formed into molybdenum, the absorbing part is formed into graphite, and the heat reflection and absorption differences of the molybdenum area and the graphite area in the circumferential direction of the crucible 2, which are contained in the opposite surfaces of the heat preservation structure 4 and the crucible 2, are adjusted, so that different parts of the heat preservation structure 4 have different heat preservation performances, and the temperature of the furnace chamber 11 is finely adjusted.
In some embodiments, the reflective portion may be a molybdenum plate or a molybdenum layer coated on the outer layer of the thermal insulation member 41 or the conditioning member 42, and the absorptive portion may be a graphite plate or a graphite layer coated on the outer layer of the thermal insulation member 41 or the conditioning member 42.
In some embodiments of the present invention, the thermal insulation member 41 and the adjustment member 42 each include: the furnace chamber comprises a first connecting part and a second connecting part which are arranged at intervals along the axial direction of the furnace chamber 11, and a plurality of main body parts which are arranged between the first connecting part and the second connecting part, wherein the first connecting part and the second connecting part are both annular, and the main body parts are connected and arranged along the circumferential direction of the first connecting part and the second connecting part. From this, fixed reflection part and absorption portion that can be stable avoid reflection part and absorption portion to take place not hard up, have guaranteed insulation construction 4's stability, have prolonged insulation construction 4's life.
In some embodiments of the present invention, as shown in fig. 1, the single crystal growth furnace 100 further comprises: and the guide cylinder is arranged in the furnace chamber 11 in a cylindrical shape and is positioned above the molten liquid, and the crystal bar pulled by the pulling mechanism penetrates through the guide cylinder in the vertical direction and extends into the crucible 2. Therefore, the single crystal growth furnace 100 has a simple overall structure, is convenient to assemble, and has uniform crystal growth.
In some embodiments of the present invention, the single crystal growth furnace 100 further comprises: and the driving mechanism is connected with the heat preservation piece 41 and/or the adjusting piece 42 and drives the heat preservation piece 41 and the adjusting piece 42 to rotate relatively. Specifically, the adjusting member 42 may be driven to rotate, the heat retaining member 41 may also be driven to rotate, and the adjusting member 42 and the heat retaining member 41 may also be driven to rotate relatively.
In one embodiment of the present invention, the crucible 2 includes a quartz crucible 212 and a graphite crucible 222.
In one embodiment of the present invention, the single crystal growth furnace 100 further comprises: and a transverse magnetic field applying device for applying a transverse magnetic field to the molten liquid in the crucible 2. The horizontal magnetic field (HMCZ) can inhibit the fluctuation of the surface of molten steel caused by thermal convection in the conventional CZ method (CZ), inhibit longitudinal thermal convection, and reduce the average temperature of molten steel after application. However, in the process of applying the transverse magnetic field, the magnetic lines of force of the magnetic field pass through the silicon melt in the quartz crucible from one end to the other end in parallel, and the lorentz force generated by the rotating silicon melt is different everywhere in the circumferential direction, so that the flow and the temperature distribution of the silicon melt are not uniform in the circumferential direction.
The heat preservation piece in the single crystal growth furnace disclosed by the embodiment of the invention is provided with the reflection part and the absorption part with different heat reflection coefficients, the heat reflection coefficient of the heat preservation device in the transverse magnetic field direction is adjustable to be lower than that in the direction vertical to the transverse magnetic field, and the temperature distribution in the molten liquid is adjusted, so that the crystal growth speed is more uniform, and the crystal growth defects are reduced. Further, for the heat preservation member comprising the heat preservation member 411 and the adjusting member 412 which can rotate relatively, the areas of the reflection part and the absorption part in the heat preservation member can be adjusted to correspond to different magnetic field strengths and magnetic field ranges. For example, if the magnetic field strength of the transverse magnetic field is large and the magnetic field range is wide, the rotatable heat retaining member 411 and the adjustment member 412 adjust the area of the absorption portion of the heat retaining member in the transverse magnetic field direction to be larger than the area of the reflection portion, and the area of the reflection portion in the direction perpendicular to the transverse magnetic field to be larger than the area of the absorption portion.
According to the crystal growth method of the single crystal growth furnace 100 according to the embodiment of the second aspect of the present invention, the crystal is grown by using the single crystal growth furnace 100 according to the embodiment of the first aspect of the present invention, and the crystal growth method includes: the adjusting member 42 is controlled to rotate relative to the heat insulating member 41, and the area of the opposite surface of the heat insulating member 41 and the heater 3 is adjusted, thereby adjusting the temperature in the furnace chamber 11
Further, the single crystal growth furnace 100 includes: a transverse magnetic field applying device provided in the furnace chamber 11 for applying a transverse magnetic field to the molten steel in the crucible 2, the crystal growth method further comprising: and controlling the relative positions of the heat preservation structure 4 and the transverse magnetic field according to the direction of the transverse magnetic field, so that the heat reflection coefficient of the heat preservation structure 4 in the direction parallel to the transverse magnetic field is smaller than the heat reflection coefficient of the heat preservation structure 4 in the direction perpendicular to the transverse magnetic field.
As described above, the direction of the transverse magnetic field can be set in the transverse magnetic field applying device. The relative position of the heat preservation member 41 and the adjusting member 42 in the heat preservation structure 4 can be controlled by driving the rotating device, and the parameters such as the speed and the angle of rotation can be set. Controlling the relative position of the insulation structure 4 and the transverse magnetic field comprises: controlling the relative positions of the heat insulating member 41 and the adjusting member 42 in the heat insulating structure 4; the relative position of the overall insulation structure 4 and the transverse magnetic field is controlled.
In one embodiment, if the thermal insulation member 41 includes a reflection portion and an absorption portion, and the adjustment member 42 includes a reflection portion and a hollow portion, the reflection portion in the adjustment member 42 and the reflection portion in the thermal insulation member 41 are adjusted to correspond, and the whole thermal insulation structure 4 is adjusted such that the absorption portion is disposed in a direction parallel to the transverse magnetic field and the reflection portion is disposed in a direction perpendicular to the transverse magnetic field.
If the thermal insulation member 41 includes a reflection portion and an absorption portion, and the adjustment member 42 includes an absorption portion and a hollow portion, the absorption portion in the adjustment member 42 corresponds to the absorption portion in the thermal insulation member 41, and the whole thermal insulation structure 4 is adjusted such that the absorption portion is disposed in a direction parallel to the transverse magnetic field and the reflection portion is disposed in a direction perpendicular to the transverse magnetic field.
Further, the temperature difference produced in the circumferential direction of the crucible 2 by the heat retaining structure 4 forms a first eddy current in the melt in the crucible 2, and the transverse magnetic field forms a second eddy current in the melt in the crucible in the direction of the vertical magnetic field, the first eddy current and the second eddy current having opposite directions.
The side heat-insulating structure and the bottom heat-insulating structure can both influence molten soup in the crucible by reflection or absorption difference of heat generated by the heater to generate eddy current. The melt eddy current caused by the heat-insulating structure can balance the melt eddy current caused by the transverse magnetic field, so that the melt is warmer, the stability of a solid-liquid interface is improved, the problem of impurity segregation is avoided, and the problems of uneven crystal growth and uneven oxygen content in a crystal bar are solved.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; the connection can be mechanical connection, electrical connection or communication; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.