CN101967675B - Device for manufacturing single crystal ingots - Google Patents
Device for manufacturing single crystal ingots Download PDFInfo
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- CN101967675B CN101967675B CN201010532816.0A CN201010532816A CN101967675B CN 101967675 B CN101967675 B CN 101967675B CN 201010532816 A CN201010532816 A CN 201010532816A CN 101967675 B CN101967675 B CN 101967675B
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- single crystal
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Abstract
The invention discloses a device for manufacturing single crystal ingots. The device comprises a main body, a crucible, a main heater, a seed crystal chuck, a heat exchanger and a first heat insulation component, wherein the crucible is arranged in the main body; the main heater is arranged around the crucible; the seed crystal chuck is positioned above the crucible and used for clamping seed crystal; the heat exchanger is positioned between the top of the crucible and the seed crystal chuck, the seed crystal chuck passes through the heat exchanger in a lifting mode, and a cooling medium for cooling the seed crystal is introduced into the heat exchanger; and the first heat insulation component is arranged between the heat exchanger and the crucible. According to the device for manufacturing the single crystal ingots, the fluid for heat exchange can be introduced into the heat exchanger from the outside of the main body to control the heat exchange in the crucible so as to control directional solidification of partial melted seed crystal and melted fed material and realize full utilization of the fluid such as helium.
Description
Technical field
The present invention relates to single crystal rod and manufacture field, particularly relate to a kind of device of manufacturing sapphire single-crystal ingot.
Background technology
Existing, utilize in the device that kyropoulos manufactures sapphire single-crystal ingot, because sapphire feed can produce microbubble in melting process.The microbubble producing is by the outside surface floating of the sapphire crystal ingot in growth.But utilize in the device of existing manufacture sapphire single-crystal ingot, the speed of growth on the top of sapphire crystal ingot is very fast, thereby cause the crystal that bubble floating has been solidified to stop, be difficult for discharging, thereby cause easy micro-bubble and the related defects of forming in sapphire single-crystal ingot.
In addition, in the device of existing manufacture sapphire single-crystal ingot, also easily there is the mutually bonding problem in sapphire single-crystal ingot and crucible periphery and bottom, thereby bring adverse influence to the growth of sapphire single-crystal ingot.
Summary of the invention
The present invention is intended at least solve one of technical problem existing in prior art.For this reason, the present invention need to provide a kind of device of manufacturing single crystal rod, and described device can improve the quality of sapphire single crystal rod for example and make full use of the utilising efficiency of cooling fluid.
Device according to manufacture single crystal rod of the present invention, comprising: main body; Be arranged on the crucible in described main body; Primary heater, described primary heater is arranged on the surrounding of described crucible, for melting the feed being contained in crucible; Seed chuck, described seed chuck is positioned on described crucible, for clamping seed crystal; Heat exchanger, described heat exchanger is between the top and seed chuck of described crucible, and described seed chuck is liftably through passing into heat-eliminating medium to carry out cooling to described seed crystal in described heat exchanger and described heat exchanger; With the first heat preservation component, described the first heat preservation component is arranged between described heat exchanger and described crucible.
According to the device of manufacture single crystal rod of the present invention, by utilizing described heat exchanger, can by outside main body by the Fluid Circulation for heat exchange be passed into and in described heat exchanger, control the heat exchange in described crucible, controlling the directional freeze of the seed crystal of described partial melting and the feed of fusing, thus the making full use of of fluid of having realized helium for example.
In addition, the device of manufacture single crystal rod according to the above embodiment of the present invention can also have following additional technical characterictic:
According to one embodiment of present invention, the first heat preservation component is heat reflection screen and/or thermal insulation layer.Heat reflection screen is for returning in crucible and save energy from the reflect heat of crucible, and the heat that thermal insulation layer also can prevent crucible is by dissipation.
According to one embodiment of present invention, under described the first heat preservation component, be provided with auxiliary heater.Auxiliary heater is used in the starting stage that forms single crystal rod and heats to prevent single crystal rod hypertrophy in a lateral direction, simultaneously also in order to prevent local overcooling.That is, by controlling this auxiliary heater, also can control the transversely crystallization velocity of direction of single crystal rod.
According to one embodiment of present invention, the temperature field that described the first heat preservation component and auxiliary heater produce is controlled in the starting stage of crystal growth the single crystal growing speed making towards the sidewall of crucible and is less than along the longitudinal downward single crystal growing speed.Thereby the starting stage single crystal rod transverse growth in crystal growth is few, the floating that is conducive to bubble in melt is discharged, and has reduced bubble and the related defects in crystal, has realized the good growth of single crystal rod.
According to one embodiment of present invention, the device of described manufacture single crystal rod further comprises: temperature control parts, described temperature control parts are arranged on the bottom center of described crucible.
Wherein, described temperature control parts are temperature tunable heaters, with the process forming single crystal rod, heat to prevent that single crystal rod from bonding to the bottom of crucible.
According to one embodiment of present invention, the device of described manufacture single crystal rod further comprises: weighting unit, described weighting unit is connected to described seed chuck, for taking the weight of crystal, described temperature control parts and/or the detected result of described primary heater based on weighting unit are controlled heating and are received crucible bottom and/or sidewall and when generation is bonding, melt the monocrystalline that is bonded to described crucible to prevent single crystal sticky.
According to one embodiment of present invention, the device of described manufacture single crystal rod further comprises: the second heat preservation component, and described the second heat preservation component is arranged between described primary heater and described main body; The 3rd heat preservation component, described the 3rd heat preservation component is located between described crucible bottom and described main body.
Alternatively, described the second heat preservation component is heat reflection screen and/or thermal insulation layer, and described the 3rd heat preservation component is heat reflection screen and/or thermal insulation layer.Wherein heat reflection screen can go back the reflect heat radiating from crucible and well heater; The heat that thermal insulation layer also can prevent crucible, by dissipation, to prevent that crystals from forming excessive thermograde, thereby makes in crystallisation process, and single crystal rod can be not bonding with the inwall of crucible, and the internal stress of crystal is also controlled.
Wherein, described heat reflection screen is formed by tungsten, molybdenum, miramint or graphite, and described thermal insulation layer is formed by heat preservation carbon felt.
According to one embodiment of present invention, described heat-eliminating medium is water or helium.
According to one embodiment of present invention, described primary heater is formed by tungsten, molybdenum, miramint or graphite.
According to one embodiment of present invention, described single crystal rod is sapphire crystal ingot.
According to the device of manufacture single crystal rod of the present invention, the starting stage formation control crystal longitudinal growth speed of growing at crystal by the first heat preservation component and auxiliary heater is higher than the temperature gradient field of transverse growth speed, and prevent that by temperature control parts single crystal rod from bonding to the bottom of crucible, thereby realized the good growth of described single crystal rod, reduced the bubble in crystal, improved the quality of described sapphire single-crystal ingot, and extracted conveniently.
Additional aspect of the present invention and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage accompanying drawing below combination obviously and is easily understood becoming the description of embodiment, wherein:
Fig. 1 is the structural representation of the device of manufacture single crystal rod according to an embodiment of the invention; And
Fig. 2 is the part-structure schematic diagram of the interior growing single-crystal ingot of crucible in Fig. 1.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of identical or similar functions from start to finish.Below by the embodiment being described with reference to the drawings, be exemplary, only for explaining the present invention, and can not be interpreted as limitation of the present invention.
In description of the invention, term " on ", orientation or the position relationship of the indication such as D score, 'fornt', 'back', " left side ", " right side ", " top ", " end " be based on orientation shown in the drawings or position relationship, be only the present invention for convenience of description rather than require the present invention with specific orientation structure and operation, therefore can not be interpreted as limitation of the present invention.
Describe below with reference to accompanying drawings according to the device of the manufacture single crystal rod of the embodiment of the present invention, wherein Fig. 1 is the structural representation of the device of manufacture single crystal rod according to an embodiment of the invention.In addition, will take that to manufacture sapphire single-crystal ingot be example in following, describe the device of manufacturing single crystal rod.
But; it should be noted that, the device of manufacture single crystal rod of the present invention also can utilize the monocrystalline of manufacturing other types, such as silicon single-crystal, oxide compound (as yttrium aluminium garnet YAG etc.) monocrystalline etc.; be for exemplary purposes herein, rather than in order to limit the scope of the invention.
As Figure 1-Figure 2, according to the device of the manufacture single crystal rod of the embodiment of the present invention, comprise main body 1, crucible 2, primary heater 3, seed chuck 4, heat exchanger 5 and the first heat preservation component 71, wherein crucible 2 is arranged in main body 1.
In the device 100 of above-mentioned manufacture sapphire single-crystal ingot; main body 1, crucible 2 etc. can form cylindrical; but it should be noted that; main body 1, crucible 2 etc. also can form other shape; such as cuboid etc.; be for purposes of illustration herein, rather than in order to limit the scope of the invention.Be understandable that, main body 1 is interior can accommodate a plurality of primary heaters 3.
Thus, by utilizing heat exchanger 5, can be by the heat-eliminating medium for heat exchange being for example passed into water or circulated helium to the interior heat exchange of controlling in crucible 2 of heat exchanger 5 outside main body 1, with the directional freeze of the seed crystal of control section fusing and the feed of fusing, and the making full use of of heat-eliminating medium of having realized water for example or helium.
In one embodiment of the invention, the first heat preservation component 71 is arranged between heat exchanger 5 and the top of crucible 2.Alternatively, the first heat preservation component 71 is heat reflection screen, and as depicted in figs. 1 and 2, heat reflection screen 7 is for returning the interior saving energy of crucible 2 from the reflect heat of crucible 2.Certainly, the first heat preservation component 71 can be also thermal insulation layer, with the heat that prevents crucible by dissipation.Further, under the joint effect of the heat exchange action of heat exchanger 5 and the insulation effect of the first heat preservation component 71, in crucible, the Transverse Temperature Gradient of melt is little, thereby make as shown in Figure 2 single crystal rod transversely the crystallization velocity of direction be less than crystallization velocity in a longitudinal direction, described single crystal rod was roughly grown along vertical direction in the starting stage of crystallization, few in the starting stage single crystal rod transverse growth of crystal growth, bubble in melt can be easily floats and discharges crucible along the outside surface of single crystal rod, therefore improved the quality of the single crystal rod of institute's crystallization.
In another embodiment of the present invention, under the first heat preservation component 71, be provided with auxiliary heater 8.As depicted in figs. 1 and 2, auxiliary heater 8 is used in the starting stage heating of single crystal growing, with prevent single crystal rod in starting stage of growth in hypertrophy in a lateral direction, simultaneously also in order to prevent local overcooling.That is, by controlling this auxiliary heater 8, also can control the transversely crystallization velocity of direction of single crystal rod.In some of them example of the present invention, the temperature field that auxiliary heater produces can be controlled in the starting stage of single crystal growing the single crystal growing speed making towards the sidewall of crucible 2 and be less than greatly along the longitudinal downward single crystal growing speed, the crystal shape generating as shown in Figure 2, this crystal shape is very beneficial for the floating of bubble in melt and discharges, thereby has promoted the quality of single crystal rod.When the growth of the bottom of crystal approaches crucible bottom, enter the middle and later periods of single crystal growing, reduce gradually the power of auxiliary heater 8 until stop heating, the transverse growth of crystal is slowly carried out gradually, thereby realized the good growth of single crystal rod.
In one embodiment of the invention, the device of manufacturing single crystal rod further comprises weighting unit, weighting unit 9 is connected to seed chuck 4, for taking the weight of crystal, and according to the heating of weighing results control temperature control parts 6 and primary heater 3, the heating power of adjusting temperature control parts 6 and primary heater 3 according to the variation of crystal weight, makes crucible bottom and sidewall keep suitable thermograde, and prevents that seed crystal is bonded to bottom and the sidewall of crucible 2.If while being bonded on the bottom of crucible 2 or sidewall in the process of single crystal rod crystallization, this weighting unit 9 just can detect the unexpected variation of crystal weight, thereby Trig control signal, make temperature control parts 6 and/or primary heater 3 be controlled heating based on detected result crucible is heated, to melt the monocrystalline that is bonded to crucible 2.In an example of the present invention, weighting unit 9 is located at outside main body 1, for example seed chuck 4 longitudinally directly over.And in another example of the present invention, weighting unit 9 also can be located at the top of the interior crucible 2 of main body 1, be for example located at seed chuck 4 longitudinally directly over.
In one embodiment of the invention, the device of manufacturing single crystal rod further comprises the second heat preservation component 72 and the 3rd heat preservation component 73, as shown in Figure 1.The second heat preservation component 72 is arranged between primary heater 3 and main body 1, that is to say, the second heat preservation component 72 is centered around the periphery of primary heater 3.The 3rd heat preservation component 73 is located between crucible 2 bottoms and main body 1.
In an example of the present invention, the second heat preservation component 72 and the 3rd heat preservation component 73 can be heat reflection screen.Heat reflection screen can be used for reflecting crucible 2 and primary heater 3 to extraradial heat, and wherein heat reflection screen separates predetermined distance with the outside surface of crucible 2 and primary heater 3, and this heat reflection is shielded and the reflect heat radiating from crucible 2 and well heater can be gone back.
In another example of the present invention, the second heat preservation component 72 and the 3rd heat preservation component 73 can be thermal insulation layer, for the sidewall of crucible 2 and bottom are incubated, thereby make in crystallisation process, single crystal rod can be not bonding with the bottom of crucible.In addition, the heat that this thermal insulation layer also can prevent crucible 2 is by dissipation, to prevent that crystals from forming excessive thermograde.
Certainly, the present invention is not limited to this.Be understandable that, the second heat preservation component 72 and the 3rd heat preservation component 73 must not be same heat reflection screen or thermal insulation layers, in some of them example of the present invention, the second heat preservation component 72 can be the heat reflection that is centered around crucible 2 surroundings and shields to reflect the heat giving off from crucible, and the 3rd heat preservation component 73 can be the heat that thermal insulation layer prevents that crucible bottom dissipation from going out.Certainly, in other example of the present invention, the second heat preservation component 72 can be the thermal insulation layer that is centered around crucible 2 surroundings, and the 3rd heat preservation component 73 can be heat reflection screen.Further be understandable that, the second heat preservation component 72 and the 3rd heat preservation component 73 can also be heat reflection screen and the thermal insulation layers after combination.
The heat reflection screen of mentioning in the foregoing description can be formed by tungsten, miramint or graphite, and thermal insulation layer is formed by heat preservation carbon felt.
In some embodiments of the invention, seed chuck 4 is 5-10rpm in the speed of rotation in seeding stage, its pulling speed is 0.01-0.4 milli m/h, in the crystallisation process of seed crystal, seed chuck upwards promotes gradually from fast to slow, thereby can make single crystal rod form single crystal growing better quality more evenly and longitudinally.
According to one embodiment of present invention, described primary heater 3 is formed by tungsten, molybdenum, miramint or graphite.
The process of manufacturing sapphire single-crystal ingot is simply described below with reference to Fig. 1-Fig. 2.
First sapphire polycrystalline feed is put in crucible, and to vacuumizing in main body 1, then utilized primary heater 3 to carry out material.After material completes, enter the seeding stage, now seed crystal, through heat exchanger 5, enters melt, realizes seed crystal partial melting.Now fluid is passed in heat exchanger 5, and the flow velocity of fluid become to keep described seed crystal by partial melting at material stage control, and make seed chuck 4 with the speed rotation of 5-10rpm, and upwards promote gradually, to control the seeding process of seed crystal.
The directional solidification growth of beginning crystal after seeding completes, in the starting stage of crystal growth, the temperature field of auxiliary heater can be controlled to and make towards the single crystal growing speed of the sidewall of crucible 2, much smaller than single crystal growing speed along the longitudinal, to heat to prevent that single crystal rod longitudinal growth is to the bottom that is bonded to crucible 2 by temperature control parts 6 in the process that forms single crystal rod simultaneously.When the growth of the bottom of crystal approaches crucible bottom, enter the middle and later periods of single crystal growing, now reduce gradually the power of auxiliary heater 8 until stop heating, the transverse growth of crystal is slowly carried out gradually, thereby realized the good growth of single crystal rod.
After single crystal rod completes, insulation is to reduce crystal internal stress, and then Slow cooling is come out of the stove.
As mentioned above, according to the device of manufacture single crystal rod of the present invention, by utilizing described heat exchanger 5, can by outside main body 1 by the Fluid Circulation for heat exchange be passed into the interior heat exchange of controlling in described crucible 2 of described heat exchanger 5, controlling the directional freeze of the seed crystal of described partial melting and the feed of fusing, thus the making full use of of fluid of having realized helium for example.In addition, temperature gradient field by auxiliary heater formation control crystal longitudinal growth speed higher than transverse growth speed, and prevent that by temperature control parts single crystal rod from bonding to the bottom of crucible 2, thereby realized the good growth of described single crystal rod, improved the quality of described sapphire single-crystal ingot, and extracted conveniently.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, the schematic statement of above-mentioned term is not necessarily referred to identical embodiment or example.And the specific features of description, structure, material or feature can be with suitable mode combinations in any one or more embodiment or example.
Although illustrated and described embodiments of the invention, those having ordinary skill in the art will appreciate that: in the situation that not departing from principle of the present invention and aim, can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claim and equivalent thereof.
Claims (13)
1. a device of manufacturing single crystal rod, is characterized in that, comprising:
Main body;
Be arranged on the crucible in described main body;
Primary heater, described primary heater is arranged on the surrounding of described crucible, for melting the feed being contained in crucible;
Seed chuck, described seed chuck is positioned on described crucible, for clamping seed crystal;
Heat exchanger, described heat exchanger is between the top and seed chuck of described crucible, and described seed chuck is liftably through passing into heat-eliminating medium to carry out cooling to described seed crystal in described heat exchanger and described heat exchanger; With
The first heat preservation component, described the first heat preservation component is arranged between described heat exchanger and described crucible.
2. the device of manufacture single crystal rod according to claim 1, is characterized in that, the first heat preservation component is heat reflection screen and/or thermal insulation layer.
3. the device of manufacture single crystal rod according to claim 2, is characterized in that, under described the first heat preservation component, is provided with auxiliary heater.
4. the device of manufacture single crystal rod according to claim 3, it is characterized in that, the temperature field that described auxiliary heater produces is controlled in the starting stage of crystal growth the single crystal growing speed making towards the sidewall of crucible and is less than along the longitudinal downward single crystal growing speed.
5. the device of manufacture single crystal rod according to claim 1, is characterized in that, further comprises:
Temperature control parts, described temperature control parts are arranged on the bottom center of described crucible.
6. the device of manufacture single crystal rod according to claim 5, is characterized in that, described temperature control parts are temperature tunable heaters.
7. the device of manufacture single crystal rod according to claim 5, is characterized in that, further comprises:
Weighting unit, described weighting unit is connected to described seed chuck, for taking the weight of crystal, described temperature control parts and/or the detected result of described primary heater based on weighting unit are controlled heating and are received crucible bottom and/or sidewall and when generation is bonding, melt the monocrystalline that is bonded to described crucible to prevent single crystal sticky.
8. the device of manufacture single crystal rod according to claim 1, is characterized in that, further comprises:
The second heat preservation component, described the second heat preservation component is arranged between described primary heater and described main body;
The 3rd heat preservation component, described the 3rd heat preservation component is located between described crucible bottom and described main body.
9. the device of manufacture single crystal rod according to claim 8, is characterized in that, described the second heat preservation component is heat reflection screen and/or thermal insulation layer, and
Described the 3rd heat preservation component is heat reflection screen and/or thermal insulation layer.
10. according to the device of the manufacture single crystal rod described in claim 2 or 9, it is characterized in that, described heat reflection screen is formed by tungsten, molybdenum, miramint or graphite, and described thermal insulation layer is formed by heat preservation carbon felt.
The device of 11. manufacture single crystal rods according to claim 1, is characterized in that, described heat-eliminating medium is water or helium.
The device of 12. manufacture single crystal rods according to claim 1, is characterized in that, described primary heater is formed by tungsten, miramint or graphite.
The device of 13. manufacture single crystal rods according to claim 1, is characterized in that, described single crystal rod is sapphire crystal ingot.
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Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102168920B (en) * | 2011-04-15 | 2012-09-26 | 中磁科技股份有限公司 | Crucible cooling device in vacuum induction melting furnace |
CN102268731A (en) * | 2011-07-12 | 2011-12-07 | 协鑫光电科技(张家港)有限公司 | Temperature field system for crystal growth |
CN103121104A (en) * | 2011-11-21 | 2013-05-29 | 高殿斌 | Production method used for vacuum crystallization furnace heat preservation assembly materials |
CN102560655A (en) * | 2012-02-29 | 2012-07-11 | 郭宏鹤 | Sapphire crystal growing furnace |
CN104451879A (en) * | 2014-11-24 | 2015-03-25 | 河南晶格光电科技有限公司 | Sapphire ingot production process |
CN106835278A (en) * | 2017-01-13 | 2017-06-13 | 许昌天戈硅业科技有限公司 | A kind of crystal growth furnace heater and sapphire crystal growing furnace |
CN106868594A (en) * | 2017-01-13 | 2017-06-20 | 许昌天戈硅业科技有限公司 | A kind of low energy consumption sapphire crystal growing furnace |
CN109695055A (en) * | 2019-03-11 | 2019-04-30 | 苏州新美光纳米科技有限公司 | Long crystal furnace and crystal system |
CN113699583B (en) * | 2021-09-28 | 2023-11-03 | 秦皇岛市和易科技有限公司 | Crystal growth method based on power reduction method |
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