CN104328483A - Single crystal growth method and device - Google Patents
Single crystal growth method and device Download PDFInfo
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- CN104328483A CN104328483A CN201410638863.1A CN201410638863A CN104328483A CN 104328483 A CN104328483 A CN 104328483A CN 201410638863 A CN201410638863 A CN 201410638863A CN 104328483 A CN104328483 A CN 104328483A
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Abstract
The invention relates to a single crystal growth method and device. The device comprises a charging part, a single crystal growth part, a heating unit and a melting unit. At the beginning, only part of seed crystals or part of seed crystals and a small amount of preloaded material are completely molten to form a molten zone at the single crystal growth part. In the single crystal growth process, the raw material is gradually added into the molten zone in a solution mode from above the molten zone, and the relative position between the heater and seed crystals is changed, so that the molten zone moves upwards relative to the seed crystals until the seed crystals grow into the single crystals with required dimensions. The material is added in the solution mode, thereby facilitating the respective control on the raw material melting and solution crystallization; and free regulation can be performed within a wide range according the optimum conditions for crystallization, thereby being beneficial to enhancing the single crystal growth speed, improving the single crystal quality and accurately controlling the single crystal components and also being beneficial to energy saving.
Description
Technical field
The invention belongs to single crystal preparation technical field, particularly relate to a kind of method for monocrystal growth and device thereof.
Background technology
Single crystal has excellent laser physics performance, and it is widely used in technical field of solid laser, as the plant and instrument such as laser ranger, lidar; High precision silicon single crystal is also the basic material of semiconductor element.The single crystal how obtaining large size or distributed components is at low cost the target that those skilled in the art pursue.
Summary of the invention
The object of the invention is to find a kind of method that can obtain distributed components, self-consistent large size single crystal.By finding the analysis of existing technique: existing growing zone-melting monocrystal method is all need to take into account fusing solid feed and liquation crystallization, is thus limited to very much simultaneously.In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of single-crystal growing apparatus, comprise reinforced portion, single crystal growing portion and heating unit, the melt device that Solid raw materials is melted is provided with between described reinforced portion and single crystal growing portion, bottom or the bottom of described melt device are provided with liquid-leaking nozzle, the Solid raw materials of melt device is entered by reinforced clan, after heating unit heats fusing, instill with the form of liquation or flow in the melting zone in single crystal growing portion, participating in single crystal growing as the raw material added.
Further, described heating unit comprises the primary heater of the described single crystal growing portion of heating and heating melt device; Or comprise the secondary heater of primary heater and the heating melt device heating described single crystal growing portion; Or comprise the primary heater of the described single crystal growing portion of heating and heating melt device and the secondary heater of heating melt device.
Further, described single crystal growing subordinate portion is provided with push rod, and push rod drives single crystal growing portion to move up and down; Or/and described primary heater is provided with running gear, heating unit is driven to move up and down.
Further, in described single crystal growing portion, being also provided with agitator, promoting melting zone component homogenizing by stirring.
Further, described liquid-leaking nozzle is one or more apertures of the latus rectum 1-10 millimeter that melt device bottom or bottom are offered; Or bottom is set to netted.
Further, described melt device is made up of dystectic, that chemical reaction does not occur relative to described liquation material.
Further, described material is the one in platinum, iridium, tungsten, molybdenum, tantalum, niobium, quartz or graphite.
Present invention also offers the method for monocrystal growth that a kind of single-crystal growing apparatus is implemented, said method comprising the steps of:
1) bottom single crystal growing portion, seed crystal is installed;
2) particulate state or Powdered Solid raw materials are put into feeder;
3) by heating unit heats seed crystal, until the fusing of described seed crystal upper end portion, in formation melting zone, seed crystal top;
4) described heating unit moves up relative to seed crystal according to single crystal growing speed, or single crystal growing portion moves down according to single crystal growing speed, and described melting zone is moved relative on seed crystal, and described monocrystalline starts growth;
5) in the process of single crystal growing, by feeder by the Solid raw materials in feeder by described monocrystalline the speed of growth needed for, be delivered to the melt device of below;
6) Solid raw materials falling into melt device forms liquation by heating unit heats, instills or flow into described melting zone, participates in described single crystal growing as the raw material added;
7), after growing up to the monocrystalline of desired size, stop growing process.
Further, completing steps 1) after, at the appropriate raw material of seed crystal top pre-add, the raw material of institute's pre-add can from step 2) in raw material identical, also can be different.
Further, described heating unit is provided with primary heater, for heating single crystal growing portion and melt device; Or increase and be provided with secondary heater, described primary heater, for heating single crystal growing portion or heating single crystal growing portion and melt device, described secondary heater only heats melt device; The type of heating that described heating unit adopts is any one of induction heating, resistive heating or radiation heating, or adopts different heating mode combined heated.
Further, the described monocrystalline of generation is pure component monocrystalline, the monocrystalline of doping and the monocrystalline of off-congruent growth.
Further, described monocrystalline is the one of aluminum oxide, doping or plain yttrium aluminum garnet, stoichiometric proportion lithium niobate or silicon single crystal.
Further, the lift velocity in described melting zone is 0.1 milli m/h-20 millis m/h.
Owing to adopting liquation to feed in raw material, melting zone need not be taken into account fusing solid feed and liquation crystallization simultaneously, freely can adjust within a large range according to the top condition of crystallization needs, obtains higher-quality monocrystalline.Meanwhile, due to thinner melting zone can be adopted and adopt agitator, be conducive to improving mass transfer condition; And the heater element power heating thinner melting zone needs can reduce, thermo-efficiency is improved, and reduces the energy consumption in production, saves mass energy; Moreover adopt the heating unit of lower-wattage, produce less energy consumption, the lagging material of needs etc. also can reduce, and are conducive to the miniaturization of equipment.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification sheets, with embodiments of the invention jointly for explaining the present invention, is not construed as limiting the invention.
Fig. 1 is the structural representation of single-crystal growing apparatus of the present invention;
In figure: 1, feeder; 2, agitator; 3, well heater; 4, melt device; 5, liquation drips; 6, induction coil; 7, crucible; 8, melting zone; 9, monocrystalline; 10, seed crystal; 11, lagging material.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
The device of following embodiment is substantially identical, describes in detail no longer one by one in an embodiment.
embodiment 1:
As shown in Figure 1, in the present embodiment, single-crystal growing apparatus comprises feeder 1, agitator 2, well heater 3, melt device 4, crucible 7 and forms the lagging material 11 of incubation cavity.Feeder 1 is positioned at the top of device, and the bottom of feeder 1 is provided with feeder, controls Solid raw materials output speed by control device.Be provided with melt device 4 below feeder, feeder 1 is communicated with by carrier pipe with melt device 4, crucible 7 upper opening, and melt device 4 is overlapped on the upper edge of well heater 3; When adopting resistance heating manner or other type of heating, the inner cavity top of the incubation cavity that melt device 4 frame is formed at lagging material 11.The outer peripheral having heaters 3 of crucible 7; The bottom of crucible 7 is fixed with seed crystal 10; Outside of deivce face is coated with lagging material 11, and induction coil 6 is arranged on position outside lagging material 11, corresponding with well heater 3.During concrete enforcement, also without crucible 7, only can use seed crystal clamping device.Seed crystal 10, crucible 7 or seed crystal clamping device and push rod and push rod tractor, comprise the melting zone that seed crystal 10 and melting sources generate and be called single crystal growing portion.
In device, melt device 4 is by dystectic, that chemical reaction does not occur relative to described liquation material, and such as platinum, iridium, tungsten, molybdenum, tantalum, niobium, quartz or graphite are made.
Monocrystalline growing process operates according to the following steps:
1) seed crystal 10 made by the alumina single crystal rod installing Φ 5x30 bottom molybdenum crucible 7, the phase oxidative aluminum feedstock in 10 millimeters, pre-add 20 gram particle footpath above seed crystal 10, by crucible push rod, seed crystal 10 is pushed into the lower edge of well heater 3, in the present embodiment, well heater 3 adopts induction heating mode; Well heater 3 heats melt device 4 and melting zone 8 simultaneously;
2) the phase oxidative aluminum feedstock of particle diameter 10 millimeters is put into feeder 1;
3) vacuumize and heat seed crystal 10 by well heater 3, until the upper end portion fusing of the phase oxidative aluminum feedstock of pre-add and seed crystal 10, in formation melting zone, seed crystal top 8;
4) well heater 3 is fixed, and to be moved up induction coil 6 with the speed of 5 millimeters per hour by induction coil running gear (not shown), along with single crystal growing moves up relative to seed crystal 10, make melting zone 8 is moved, monocrystalline 9 starts growth;
5) molybdenum melt device 4 is positioned at the middle and upper part of well heater 3, and this spot temperature is higher; Melting zone 8 is positioned at the below of melt device 4, and this spot temperature is relatively low, in the process that monocrystalline 9 grows, needed for the speed of growth of by feeder the Solid raw materials in feeder being pressed monocrystalline 9, adds in melt device 4;
6) in melt device 4, Solid raw materials is molten into liquation, and the aperture of the latus rectum offered by melt device 4 lower sides 10 millimeters is flowed out, and forms liquation and drips 5, and instillation or inflow melting zone 8, participate in single crystal growing as the raw material added.By controlling the feed rate of feeder, making raw material liquation add speed suitable with monocrystalline 9 speed of growth, keeping liquation feed rate and monocrystalline 9 speed of growth to balance;
7) alumina single crystal of diameter 50 millimeters, length 200 millimeters is finally grown.
Adopt aforesaid method, as shown in Figure 1, melting zone 8 thickness in single crystal growing portion can keep very thin; Meanwhile, the raw material in melt device 4 is also less; Energy required for fusing correspondingly decreases, and thermo-efficiency is improved, and reduces the energy consumption in production, saves mass energy.
embodiment 2:
In the present embodiment, single-crystal growing apparatus is substantially the same manner as Example 1, and be distinguished as device and be also provided with agitator 2, agitator 2 is arranged on the top of device, and flabellum stretches in melting zone 8 and stirs liquation, in order to make mass transfer even.The flabellum setting position of agitator needs higher than crystal plane, avoids the destruction to crystallisation process.
1) use the iridium crucible of upper internal diameter 100 millimeters, length 140 millimeters as crucible 7; The yttrium-aluminum garnet single crystal of the neodymium-doped 1%mol of Φ 10x30 rod is done the bottom that seed crystal 10 is arranged on crucible 7, the yttrium aluminum garnet powder 50 grams of pre-add neodymium-doped 5%mol above seed crystal 10, and seed crystal 10 is positioned at the lower edge of well heater 3; Well heater 3 is melting zone 8 and melt device 4 simultaneously;
2) the yttrium aluminum garnet feed particulate material of neodymium-doped 1%mol is pre-loaded into feeder 1;
3) vacuumize and heated a small amount of raw material of seed crystal 10 and pre-add by well heater 3, until described pre-add raw material and the fusing of seed crystal 10 upper end portion, in formation melting zone, seed crystal top 8;
4) well heater 3 is fixed; Move down crucible 7 by the push rod of crucible bottom with the speed of 1 millimeter per hour, then melting zone 8 moves up for seed crystal 10 along with monocrystalline 9 growth phase, and monocrystalline 9 keeps growth;
5) iridium melt device 4 is tubbiness, and frame is at the top of lagging material 11 inner chamber; Be positioned at the middle and upper part of well heater 3 bottom it, bottom melt device 4, offer the aperture of latus rectum 1 millimeter; Also iridium wire netting can be adopted as the bottom of melt device 4.In the process that monocrystalline 9 grows, needed for the speed of growth of by feeder the feed particulate material in feeder 1 being pressed monocrystalline 9, add melt device 4;
6) in melt device 4, Solid raw materials is molten into liquation, is flowed out by the mesh bottom melt device 4, forms liquation and drips 5, and instillation or inflow melting zone 8, participate in single crystal growing as the raw material added; Control the feed rate of feeder, make raw material liquation add speed suitable with monocrystalline 9 speed of growth, keep liquation feed rate and monocrystalline 9 speed of growth to balance;
7) flabellum of molybdenum agitator 2 stretches into melting zone 8, stirs liquation, makes material composition in melting zone 8 more even by stirring;
8) yttrium-aluminum garnet single crystal of neodymium-doped 1%mol of diameter 100 millimeters, length 100 millimeters is finally grown.
The mode that the present embodiment also can adopt well heater 3 rising to drive melting zone 8 to rise generates monocrystalline manner.When adopting well heater 3 rising manner, correspondingly agitator 2 is equipped with synchronous hoisting device (not shown), makes the lift velocity of agitator 2 rise identical with well heater 3, mates with the lift velocity in melting zone 8 to reach, and ensures the effect stirred.
embodiment 3:
In the present embodiment, single-crystal growing apparatus is substantially the same manner as Example 2, is distinguished as well heater 3 for resistance heater, is divided into the first resistance heater and the second resistance heater.
1) use the crucible of internal diameter 50 millimeters, length 70 millimeters of platinum as crucible 7, the chemical metering ratio lithium niobate monocrystal of Φ 10x30 rod is done the bottom that seed crystal 10 is arranged on crucible 7, the Lithium niobium trioxide powder 50 grams of the rich lithium 5%mol of pre-add above seed crystal 10, seed crystal 10 is positioned at the lower edge of resistance heater 3;
2) stoichiometric proportion lithium niobate particulate material is pre-loaded into feeder 1;
3) separately through a small amount of raw material of the first resistive heater heats seed crystal 10 and pre-add, until described raw material and the fusing of seed crystal 10 first half, in formation melting zone, seed crystal top 8;
4) resistance heater 3 is fixed; Move down crucible 7 by the push rod of crucible 7 bottom with the speed of 0.1 millimeter per hour, then melting zone 8 moves up relative to seed crystal 10, and monocrystalline 9 keeps growth;
5) platinum melt device 4 is inverted cone shape, and bottom is positioned at the middle and upper part of the second resistance heater, in the process that monocrystalline 9 grows, needed for the speed of growth of by feeder the raw material in feeder 1 being pressed monocrystalline 9, adds melt device 4;
6) in melt device 4, Solid raw materials is molten into liquation, is flowed out by the aperture of the latus rectum 5 millimeters offered bottom melt device 4, forms liquation and drips 5, and instillation or inflow melting zone 8, participate in single crystal growing as the raw material added.By controlling the feed rate of feeder, making raw material liquation add speed suitable with monocrystalline 9 speed of growth, keeping liquation feed rate and monocrystalline 9 speed of growth to balance;
7) being provided with platinum agitator 2 in crucible 7, making material composition in melting zone more even by stirring;
8) chemical metering ratio lithium niobate monocrystal of diameter 50 millimeters, length 100 millimeters is finally grown.
embodiment 4:
In the present embodiment, single-crystal growing apparatus is substantially the same manner as Example 1, is distinguished as well heater 3 for radiation heater.
1) make seed crystal 10 with the silicon single crystal bar that quartzy seed chuck fixes Φ 10x20, seed crystal 10 is positioned in a focus of oval high light radiation focal heat monocrystal growing furnace, another focus is put a strong light and makes radiant heating source;
2) pulverous high-purity polycrystalline silicon raw material is loaded feeder 1;
3) vacuumize in stove, by strong light radiation heating seed crystal 10, until the fusing of seed crystal 10 upper end portion, in formation melting zone, seed crystal top 8;
4) move down seed crystal 10 by the push rod of quartzy seed crystal clamping device bottom with the speed of 20 millimeters per hour, then melting zone 8 moves up relative to seed crystal 10, and monocrystalline 9 starts growth;
5) the quartz melt device 4 of graphite resistance heating is separately positioned at above seed crystal 10, melt device 4 lower sides has the aperture of several latus rectums 3 millimeters, in the process that monocrystalline 9 grows, needed for the speed of growth of by feeder the raw material in feeder 1 being pressed monocrystalline 9, add melt device 4;
6) in melt device 4, Solid raw materials is molten into liquation, and the aperture of the latus rectum offered by melt device 4 lower sides 3 millimeters is flowed out, and forms liquation and drips 5, and instillation or inflow melting zone 8, participate in single crystal growing as the raw material added.By controlling the feed rate of feeder, making raw material liquation add speed suitable with monocrystalline 9 speed of growth, keeping liquation feed rate and monocrystalline 9 speed of growth to balance;
7) the high quality silicon monocrystalline of diameter 10 millimeters, length 100 millimeters is finally grown.
Method for monocrystal growth of the present invention and device are last it is noted that according to the mode of embodiment, change batching, adopt corresponding technique, not only may be used for growing pure component monocrystalline (can without agitator 2) and also may be used for the monocrystalline of grow doping or the monocrystalline (adding agitator 2) of off-congruent growth.The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a single-crystal growing apparatus, comprise reinforced portion, single crystal growing portion and heating unit, it is characterized in that: between described reinforced portion and single crystal growing portion, be provided with the melt device that Solid raw materials is melted, bottom or the bottom of described melt device are provided with liquid-leaking nozzle, the Solid raw materials of melt device is entered by reinforced clan, after heating unit heats fusing, instill with the form of liquation or flow in the melting zone in single crystal growing portion, participating in single crystal growing as the raw material added.
2. single-crystal growing apparatus according to claim 1, is characterized in that: described heating unit comprises the primary heater of the described single crystal growing portion of heating and heating melt device; Or comprise the secondary heater of primary heater and the heating melt device heating described single crystal growing portion; Or comprise the primary heater of the described single crystal growing portion of heating and heating melt device and the secondary heater of heating melt device.
3. single-crystal growing apparatus according to claim 2, is characterized in that: described single crystal growing subordinate portion is provided with push rod, and push rod drives single crystal growing portion to move up and down; Or/and described primary heater is provided with running gear, heating unit is driven to move up and down.
4. single-crystal growing apparatus according to claim 1, is characterized in that: be also provided with agitator in described single crystal growing portion, promotes melting zone component homogenizing by stirring.
5. single-crystal growing apparatus according to claim 1, is characterized in that: described liquid-leaking nozzle is one or more apertures of the latus rectum 1-10 millimeter that melt device bottom or bottom are offered; Or bottom is set to netted.
6. single-crystal growing apparatus according to claim 1, is characterized in that: described melt device is made up of dystectic, that chemical reaction does not occur relative to described liquation material.
7. adopt the method for monocrystal growth that in claim 1 to 6, any one single-crystal growing apparatus is implemented, it is characterized in that, said method comprising the steps of:
1) bottom single crystal growing portion, seed crystal is installed;
2) particulate state or Powdered Solid raw materials are put into feeder;
3) by heating unit heats seed crystal, until the fusing of described seed crystal upper end portion, in formation melting zone, seed crystal top;
4) described heating unit moves up relative to seed crystal according to single crystal growing speed, or single crystal growing portion moves down according to single crystal growing speed, and described melting zone is moved relative on seed crystal, and described monocrystalline starts growth;
5) in the process of single crystal growing, by feeder by the Solid raw materials in feeder by described monocrystalline the speed of growth needed for, be delivered to the melt device of below;
6) Solid raw materials falling into melt device forms liquation by heating unit heats, instills or flow into described melting zone, participates in described single crystal growing as the raw material added;
7), after growing up to the monocrystalline of desired size, stop growing process.
8. method for monocrystal growth according to claim 7, is characterized in that: completing steps 1) after, at the appropriate raw material of seed crystal top pre-add, the raw material of institute's pre-add can with step 2) in raw material identical or different.
9. method for monocrystal growth according to claim 7, is characterized in that: described heating unit is provided with primary heater, for heating single crystal growing portion and melt device; Or increase and be provided with secondary heater, described primary heater, for heating single crystal growing portion or heating single crystal growing portion and melt device, described secondary heater only heats melt device; The type of heating that described heating unit adopts is any one of induction heating, resistive heating or radiation heating, or adopts different heating mode combined heated.
10. method for monocrystal growth according to claim 7, is characterized in that: the described monocrystalline of generation is pure component monocrystalline, the monocrystalline of doping or the monocrystalline of off-congruent growth.
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| CN105369361A (en) * | 2015-12-03 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Method and apparatus for preparing sapphire single crystals by moving thermal field |
| CN106012010A (en) * | 2016-08-15 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Method and apparatus for secondary addition of doping agent |
| CN110546314A (en) * | 2018-03-29 | 2019-12-06 | 株式会社水晶系统 | Single crystal manufacturing apparatus and single crystal manufacturing method |
| CN112176395A (en) * | 2020-10-13 | 2021-01-05 | 福建福晶科技股份有限公司 | Device and method for growing high-quality large-size BiBO crystal by molten salt growth method |
| US11326270B2 (en) | 2018-03-29 | 2022-05-10 | Crystal Systems Corporation | Single-crystal production equipment and single-crystal production method |
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