CN113913918A - Crystal growth furnace suitable for Bridgman-Stockbarge method - Google Patents
Crystal growth furnace suitable for Bridgman-Stockbarge method Download PDFInfo
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- CN113913918A CN113913918A CN202111187759.1A CN202111187759A CN113913918A CN 113913918 A CN113913918 A CN 113913918A CN 202111187759 A CN202111187759 A CN 202111187759A CN 113913918 A CN113913918 A CN 113913918A
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- 239000013078 crystal Substances 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 139
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 238000009413 insulation Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims abstract description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims description 33
- 230000008025 crystallization Effects 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 20
- 230000000903 blocking effect Effects 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 11
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002109 crystal growth method Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 229910010293 ceramic material Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 description 8
- 238000002844 melting Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000012297 crystallization seed Substances 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 229910003327 LiNbO3 Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- -1 for example Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A crystal growth furnace suitable for a crucible descending method comprises a crucible and a heat-resistant pipe arranged on a lifting platform, wherein the heat-resistant pipe is arranged in the crucible, and Al is filled in the heat-resistant pipe2O3Powder of Al2O3Wrapping the closed crucible with the powder; a heating pipe is arranged outside the heat-resistant pipe, and a heat insulation box is arranged outside the heating pipe; the crucible is connected with the crucible through a flow guide pipe, the crucible is connected with the crucible through the crucible, and the crucible is connected with the crucible; the heating ring is arranged outside the flow guide pipe, and the top of the crucible is communicated to the outside of the heat preservation box through the outlet pipe. The invention can be modified on the existing crystal growth furnace, realizes the timely discharge of the uncrystallized raw material only by arranging the flow guide pipe, and ensures that the obtained single crystal is a completely transparent whole crystal bar.
Description
Technical Field
The invention relates to the field of crystal growth furnaces, in particular to a crystal growth furnace suitable for a Bridgman-Stockbarge method.
Background
The Bridgman method as one kind of melt growing method may be used in growing stoichiometric lithium niobate monocrystal and features that: the seed crystal is arranged at the bottom of the crucible, the upper part of the seed crystal is polycrystal raw grain and is filled in the crucible, the crucible filled with raw materials is placed in a hearth, when the crucible descends continuously and slowly, the melt enters a crystallization area and is directionally crystallized into single crystal under the nucleation effect of the seed crystal, the whole melt passes through the crystallization area completely, the growth of the single crystal is finished, the temperature is reduced to a fixed temperature along with a furnace, and the crucible is peeled off to obtain a single crystal blank.
When the same-component single crystal (the melt component is consistent with the single crystal component) is grown by the conventional descent method, a completely transparent whole crystal rod can be obtained, but in practice, when a non-same-component single crystal is grown, the upper half part of the single crystal is more and more severely crystallized, mixed crystals appear, the mixed crystals are not clear, and the whole single crystal is cracked frequently, so that the single crystal growth fails.
Disclosure of Invention
In view of the problems raised by the background art, the present invention provides a crystal growth furnace to which the Bridgman-Stockbarge method is applied, and the present invention will be further described below.
A crystal growth furnace suitable for a crucible descending method comprises a crucible and a heat-resistant pipe arranged on a lifting platform, wherein the heat-resistant pipe is arranged in the crucible, and Al is filled in the heat-resistant pipe2O3Powder of Al2O3Wrapping the closed crucible with the powder; a heating pipe is arranged outside the heat-resistant pipe, and a heat insulation box is arranged outside the heating pipe; the guide pipe comprises an inner section positioned in the heat insulation box and an outer section positioned outside the heat insulation box, the inner section and the outer section are communicated, and the inner section is communicated with the crucible; the communicating part of the flow guide pipe and the crucible is used as an inflow opening, the condition of opaque crystallization is about to occur when the crystals reach the height of the inflow opening, and the height of the outflow opening of the flow guide pipe is lower than that of the inflow opening; the heating ring is arranged outside the flow guide pipe, and the top of the crucible is communicated to the outside of the heat preservation box through the outlet pipe.
Optionally, the crystal growth method using a material other than the raw material as the plugging material includes: injecting a section of molten plugging material from an outflow port outside the heat preservation box, and cooling and solidifying; injecting raw materials into the crucible through the eduction tube, and electrifying the heating tube to generate heat; gradually descending the lifting platform through a driving device, and gradually crystallizing to form a crystal bar; and after the opaque crystallization occurs, the heating ring is electrified to heat the flow guide pipe, the blocking material in the flow guide pipe is melted, and the uncrystallized raw material flows out from the communicating pipe to obtain a completely transparent crystal bar.
Preferably, the crystal growth method using the raw material as the plug, wherein the draft tube is used only as the discharge raw material and the introduction tube is used only as the injection raw material, that is, the draft tube and the flow direction of the raw material in the introduction tube have unity, comprises: injecting raw materials into the crucible through the eduction tube, and electrifying the heating tube to generate heat; after the raw material is immersed in the inflow port, the raw material is injected into the delivery pipe for a section of height, the injection of the raw material is stopped, and the raw material is continuously injected after the raw material in the delivery pipe is cooled, crystallized and blocked; gradually descending the lifting platform through a driving device, and gradually crystallizing to form a crystal bar; and after the opaque crystallization occurs, the heating ring is electrified to heat the flow guide pipe, the blocking material in the flow guide pipe is melted, and the uncrystallized raw material flows out from the communicating pipe to obtain a completely transparent crystal bar.
Preferably, the outflow port of the delivery pipe is connected with a transparent elbow pipe, the transparent elbow pipe is bent upwards, and the top of the transparent elbow pipe is higher than the inflow port of the delivery pipe but lower than the liquid level of the raw materials in the crucible during liquid drainage; when the raw material is injected, the raw material is stopped being injected when the raw material in the guide pipe rises to the transparent bent pipe and does not reach the top height, and the raw material is continuously injected after the raw material in the guide pipe is cooled, crystallized and blocked.
Preferably, the transparent elbow may be made of a transparent ceramic material that is resistant to high temperatures.
Preferably, the introducing pipe is connected with a U-shaped seal, and a heating ring is arranged outside the U-shaped seal; after injecting the raw materials, continuously injecting the raw materials into the U-shaped seal, and immersing the raw materials into the U-shaped seal to form a seal; when the raw materials need to be removed after the crystallization is finished, the heating ring is electrified and heated to melt the raw materials in the U-shaped seal, then a certain amount of raw materials are injected, the raw materials in the U-shaped seal are injected into the crucible together, and finally the raw materials flow out of the guide pipe. The crucible is ensured to maintain a sealed state in the crystallization process, and the pressure in the crucible can be kept constant when the raw materials are discharged.
Preferably, the heating ring heats the solid raw material in the U-shaped seal to be consistent with the temperature of the raw material in the crucible; then, a certain amount of raw materials are injected, the raw materials in the U-shaped seal are injected into the crucible together, the temperature of the raw materials in the crucible keeps the original temperature, and the crystallized crystal bar is not interfered.
Preferably, an air cooler is arranged and blows towards the U-shaped seal and the part of the guide pipe outside the heat insulation box; the curing time can be shortened.
Preferably, the part of the flow guide pipe outside the heat preservation box is arranged in a spiral shape; on the one hand, the contact area of the part of the flow guide pipe outside the heat preservation box and the air cooler is increased, the curing time is further shortened, and on the other hand, the plugging effect of the raw materials is guaranteed due to interaction of the cured plugging material and the pipeline.
Has the advantages that: compared with the prior art, the invention can be modified on the existing crystal growth furnace, realizes the clear effect on the raw materials which are not crystallized by only arranging the guide pipe, and ensures that the obtained single crystal is a completely transparent whole crystal bar.
Drawings
FIG. 1: the invention has a structure schematic diagram;
in the figure: crucible 1, lifting platform 2, heat-resistant pipe 3, heating pipe 4, heat preservation box 5, crystallization seeds 6, draft tube 7, heating ring 8, outlet pipe 9, inflow opening 14, transparent bent pipe 10, U-shaped seal 11, air cooler 12 and Al2O3And (3) powder 13.
Detailed Description
A specific embodiment of the present invention will be described in detail with reference to fig. 1.
A crystal growth furnace suitable for a Bridgman method comprises a crucible 1 for loading raw materials and a heat-resistant tube 3 arranged on a lifting platform 2, wherein the lifting platform 2 is lifted in the vertical direction under the action of external driving equipment, the crucible 1 is internally provided with the heat-resistant tube 3, and the heat-resistant tube 3 is filled with Al2O3Powder of Al2O3The powder wraps the closed crucible 1; heating pipe 4 is provided with outward to heat-resistant pipe 3, and heating pipe 4 generates heat after circular telegram, through the steerable power of generating heat of control current, and insulation can 5 is provided with outward to heating pipe 4, and insulation can 5 energy storage reduces heat and runs off.
The heating pipe 4 generates heat after being electrified, and the heat is transferred to Al through the heat-conducting heat-resistant pipe2O3Powder of Al2O3Powder temperature rapidly rises while Al2O3Good heat-conducting property of powder, Al2O3The powder not only has the function of supporting and stabilizing the crucible, but also heats the crucible to raise the temperature. The bottom of the crucible is provided with crystallization seeds 6, and the crystallization seeds 6 provide crystallization direction, so that the subsequent crystals have unicity. After the heating pipes are heated, a melting area for keeping the raw materials in a liquid state is arranged between the heating pipes, the lifting platform 2 vertically moves downwards under the action of external driving equipment, the lower part of the lifting platform moves out of the melting area and then enters a crystallization area, the temperature of the crystallization area is lower than that of the melting area, and the raw materials are crystallized in the crystallization area.
The above technical solution for obtaining a crystal rod by a crucible descent method in the prior art is that, in this solution, there is an unsolved risk of crystal rod cracking at the end stage of crystallization, and in the early stage of crystallization, crystallization is smooth, and the obtained crystal rod is a completely transparent whole crystal rod, but in practice, there is a deviation between the melt composition and the single crystal composition, for example, the raw material is LiNbO3However, the total composition of crystals precipitated during crystallization can be written as Li0.9-1NbO3In the later stage of crystallization, the raw material is gradually turbid, mixed crystals appear at last, the crystals are not clear, growth grains appear in the crystallization process, the crystals have internal stress and cause the whole single crystal to crack, and finally the single crystal growth fails. Based on the method, the conventional crystal growth furnace is modified to avoid the risks of crystal opaqueness and even crystal bar crack of the tail sound of the crystal.
In this embodiment, a flow guide pipe 7 is further provided, the flow guide pipe 7 comprises an inner section located in the heat insulation box and an outer section located outside the heat insulation box, the inner section and the outer section are communicated, the inner section is communicated with the crucible 1, and the flow guide pipe 7 is used for guiding out the raw material which is not crystallized yet from the flow guide pipe 7 under the condition that crystals are not transparent in the later stage of crystallization, so as to interrupt crystallization.
In the embodiment, after the draft tube 7 is introduced, the communication part of the draft tube 7 and the crucible 1 is used as the inflow port 14, the height of the inflow port needs to be set according to the amount of the raw material, and the setting can be performed according to past experience, so that the situation of opaque crystallization is about to occur when the crystallization reaches the height of the inflow port, and at the moment, the raw material which is not crystallized yet is led out to block the subsequent crystallization.
The raw material is led out and applied to the principle of a communicating vessel by a flow guide pipe, the height of an outlet of the flow guide pipe is required to be lower than that of an inlet, according to the principle, when the raw material liquid is added into a crucible, the height of the raw material liquid must exceed that of the inlet 14, at the moment, the raw material flows out of the flow guide pipe serving as the communicating vessel, and the surplus raw material is eliminated in the later period in order to block the outflow of the raw material liquid, a heating ring 8 is arranged outside the flow guide pipe 7, a certain amount of melting blocking material is led into the flow guide pipe 7 in advance before the raw material is added into the crucible, the flow guide pipe is blocked after the melting blocking material is cooled and solidified, then the raw material is added into the crucible, and after the raw material is injected and immersed into the inlet, the raw material enters the flow guide pipe and fills the residual space of the flow guide pipe, but the raw material cannot flow out due to the blocking of the flow guide pipe; and after crystallization to generate opaque crystallization, a heating ring 8 arranged outside the flow guide pipe 7 is electrified to heat the flow guide pipe, solid blocking materials in the flow guide pipe are melted, and based on the arrangement that the height of the flow outlet of the flow guide pipe is lower than that of the flow inlet, fluid raw materials flow out of the flow guide pipe under the action of pressure difference, and residual raw materials and the blocking materials flow out together until the liquid level of the raw materials reaches the flow inlet.
It should be noted that while the remaining raw material is simultaneously flushed out of the plug, the raw material also contains semi-crystalline solid, in practice, the temperature between the melting zone and the crystallization zone cannot jump, a temperature gradient zone exists, a semi-crystallization state exists in the zone, and in order to ensure that the obtained crystal rod is completely transparent and has no growth lines, the height of the inlet is set to satisfy the requirement that the fluid raw material and the semi-crystalline solid-liquid mixture are all discharged.
It is also necessary to arrange that, according to the principle of communicating vessels, the pressure difference exists at the two ends of the flow guide tube 7 on the premise of leading out the principle through the flow guide tube 7, and the crucible 1 in the prior art is coated with Al2O3The crucible is sealed, and when the raw material is discharged, the crucible in the sealed state cannot maintain the pressure difference, so in the embodiment, the top of the crucible 1 is communicated to the outside of the heat insulation box through the eduction tube 9 to maintain the constant pressure in the crucible, so that the raw material is smoothly discharged.
The melting blocking material can be raw material or other solid material with lower melting point, without limitation.
If other solid materials are adopted, the crystal growth method based on the crystal growth furnace provided by the invention comprises the following steps:
injecting a section of molten plugging material from an outflow port outside the heat preservation box, and cooling and solidifying;
injecting raw materials into the crucible through the eduction tube, and electrifying the heating tube to generate heat;
gradually descending the lifting platform through a driving device, and gradually crystallizing to form a crystal bar;
and after the crystal is not transparent and crystallized (or is reduced to a preset height), the heating ring is electrified to heat the flow guide pipe, the blocking material in the flow guide pipe is melted, and the uncrystallized raw material flows out of the communicating pipe to obtain a completely transparent crystal bar.
If the raw material is used as the plugging material, the flow guide pipe is only used for discharging the raw material and the introducing pipe is only used for injecting the raw material, that is, the flow direction of the raw material in the flow guide pipe and the introducing pipe has unicity, which is adopted as a preferred embodiment in this embodiment, the method for crystal growth based on the crystal growth furnace comprises:
injecting raw materials into the crucible through the eduction tube, and electrifying the heating tube to generate heat;
after the raw material is immersed in the inflow port, the raw material is injected into the delivery pipe for a section of height, the injection of the raw material is stopped, and the raw material is continuously injected after the raw material in the delivery pipe is cooled, crystallized and blocked;
gradually descending the lifting platform through a driving device, and gradually crystallizing to form a crystal bar;
and after the crystal is not transparent and crystallized (or is reduced to a preset height), the heating ring is electrified to heat the flow guide pipe, the blocking material in the flow guide pipe is melted, and the uncrystallized raw material flows out of the communicating pipe to obtain a completely transparent crystal bar.
The raw materials are adopted as the putty in the embodiment, through pouring into the raw materials and making it crystallize in order to block up the delivery pipe, in practice, through the height of the injection volume control injection of control raw materials in the delivery pipe, but based on the raw materials temperature height, the flow measurement degree of difficulty is big, the height of pouring into in the accessible visual control delivery pipe must not be higher than the outfall, specifically in this embodiment, the outfall of delivery pipe is connected with transparent return bend 10, transparent return bend 10 is upswept, its top is higher than the inflow mouth of honeycomb duct but is less than the liquid level height of raw materials in the crucible when flowing back, when pouring into the raw materials, when the raw materials in the delivery pipe rise to in transparent return bend 10 and do not reach the top height in the time stop pouring into the raw materials, wait to pour into the raw materials after the cooling crystallization of raw materials in the delivery pipe stops pouring into the raw materials, make the operation visual.
The transparent elbow 10 may be made of a high temperature resistant transparent ceramic material.
Further, in this embodiment, in order to ensure the stability of the crystallization process, the crucible is in a sealed state, and the implementation scheme is as follows: the introducing pipe is connected with a U-shaped seal 11 which can store a certain amount of raw materials, after the raw materials are injected, the raw materials are continuously injected into the U-shaped seal 11, the raw materials are immersed in the U-shaped seal 11 to form a seal, and the sealed state can be maintained after the raw materials in the U-shaped seal are crystallized; the heating ring is also arranged outside the U-shaped seal, when the raw materials need to be removed after the crystallization is finished, the heating ring is electrified and heated to melt the raw materials in the U-shaped seal, then a certain amount of raw materials are injected, the raw materials in the U-shaped seal are injected into the crucible together, and finally the raw materials flow out of the flow guide pipe.
In this embodiment, the heating ring heats the solid raw material in the U-shaped seal 11 to a temperature equal to the temperature of the raw material in the crucible 1, and then injects a predetermined amount of raw material into the crucible, and the temperature of the raw material in the U-shaped seal is maintained at the original temperature, so that the crystallized ingot is not disturbed.
In order to accelerate the solidification of the raw materials in the U-shaped seal 11 and the blocking materials in the flow guide pipe 7, an air cooler 12 is further arranged, and the air cooler 12 blows to the U-shaped seal and the part of the flow guide pipe outside the heat insulation box, so that the solidification time can be shortened. The air coolers 12 can be set into two independent groups or only one group, and when only one group is set, the air coolers can be arranged on the turntable structure to rotate so as to realize cooling of the U-shaped seal and the flow guide pipe respectively.
In this embodiment, the honeycomb duct is located the part outside the insulation can and sets up to the heliciform, and this sets up the area of contact that has increased the honeycomb duct and is located the part outside the insulation can and the air-cooler on the one hand, further shortens the curing time, and on the other hand, the shutoff effect to the raw materials is more guaranteed with pipeline interact to the putty after the solidification.
The embodiment is not illustrated for other auxiliary structures in the prior art, such as a thermocouple, a thermometer, and the like, and does not influence the understanding of the invention.
The invention can be modified on the existing crystal growth furnace, realizes the clear effect on the raw materials which are not crystallized by only arranging the flow guide pipe, and ensures that the obtained single crystal is a completely transparent whole crystal bar.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A crystal growth furnace suitable for a crucible descending method comprises a crucible (1) and a heat-resistant pipe (3) arranged on a lifting platform (2), wherein the crucible (1) is internally provided with the heat-resistant pipe (3), and Al is filled in the heat-resistant pipe (3)2O3Powder of Al2O3The powder wraps the closed crucible (1); a heating pipe (4) is arranged outside the heat-resistant pipe (3), and a heat-insulating box (5) is arranged outside the heating pipe (4); the method is characterized in that:
the crucible pot is characterized by further comprising a flow guide pipe (7), wherein the flow guide pipe (7) comprises an inner section positioned in the heat insulation box and an outer section positioned outside the heat insulation box, the inner section and the outer section are communicated, and the inner section is communicated with the crucible pot (1);
the communicating part of the flow guide pipe (7) and the crucible (1) is used as an inflow opening (14), the situation of opaque crystallization is about to occur when the crystals reach the height of the inflow opening, and the height of the outflow opening of the flow guide pipe is lower than that of the inflow opening;
a heating ring (8) is arranged outside the flow guide pipe (7), and the top of the crucible (1) is communicated to the outside of the heat preservation box through an outlet pipe (9).
2. The crystal growth furnace of claim 1, wherein:
the outflow port of the delivery pipe (7) is connected with a transparent elbow pipe (10), the transparent elbow pipe (10) is bent upwards, and the top of the transparent elbow pipe is higher than the inflow port of the delivery pipe but lower than the liquid level of the raw materials in the crucible during liquid discharge;
when the raw materials are injected, the raw materials are stopped being injected when the raw materials in the guide pipe rise into the transparent bent pipe (10) and do not reach the top height, and the raw materials are continuously injected after the raw materials in the guide pipe are cooled, crystallized and blocked.
3. The crystal growth furnace of claim 2, wherein:
the transparent bent pipe (10) can be made of high-temperature-resistant transparent ceramic material.
4. The crystal growth furnace of claim 2, wherein:
the lead-in pipe is connected with a U-shaped seal (11), and a heating ring is arranged outside the U-shaped seal;
after injecting the raw materials, continuously injecting the raw materials into the U-shaped seal (11), and forming a seal after the raw materials immerse the U-shaped seal (11);
when the raw materials need to be removed after the crystallization is finished, the heating ring is electrified and heated to melt the raw materials in the U-shaped seal, then a certain amount of raw materials are injected, the raw materials in the U-shaped seal are injected into the crucible together, and finally the raw materials flow out of the guide pipe.
5. The crystal growth furnace of claim 4, wherein:
the heating ring heats the solid raw material in the U-shaped seal (11) to be consistent with the temperature of the raw material in the crucible (1); then a certain amount of raw materials are injected, and the raw materials in the U-shaped seal are injected into the crucible together.
6. The crystal growth furnace of claim 4, wherein:
the air cooler (12) is also arranged, and the air cooler (12) blows towards the U-shaped seal and the part of the guide pipe outside the heat insulation box.
7. The crystal growth furnace of claim 5, wherein:
the part of the draft tube outside the heat preservation box is arranged in a spiral shape.
8. The crystal growth method of a crystal growth furnace according to claim 1, wherein a material other than the raw material is used as a plug, and the method comprises:
injecting a section of molten plugging material from an outflow port outside the heat preservation box, and cooling and solidifying;
injecting raw materials into the crucible through the eduction tube, and electrifying the heating tube to generate heat;
gradually descending the lifting platform through a driving device, and gradually crystallizing to form a crystal bar;
and after the opaque crystallization occurs, the heating ring is electrified to heat the flow guide pipe, the blocking material in the flow guide pipe is melted, and the uncrystallized raw material flows out from the communicating pipe to obtain a completely transparent crystal bar.
9. The crystal growth method in a crystal growth furnace according to claim 1, wherein the raw material is used as a plug, the flow guide tube is used only for discharging the raw material, the introduction tube is used only for injecting the raw material, and the flow direction of the raw material in the flow guide tube and the introduction tube is uniform, the method comprising:
injecting raw materials into the crucible through the eduction tube, and electrifying the heating tube to generate heat;
after the raw material is immersed in the inflow port, the raw material is injected into the delivery pipe for a section of height, the injection of the raw material is stopped, and the raw material is continuously injected after the raw material in the delivery pipe is cooled, crystallized and blocked;
gradually descending the lifting platform through a driving device, and gradually crystallizing to form a crystal bar;
and after the opaque crystallization occurs, the heating ring is electrified to heat the flow guide pipe, the blocking material in the flow guide pipe is melted, and the uncrystallized raw material flows out from the communicating pipe to obtain a completely transparent crystal bar.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111187759.1A CN113913918A (en) | 2021-10-12 | 2021-10-12 | Crystal growth furnace suitable for Bridgman-Stockbarge method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111187759.1A CN113913918A (en) | 2021-10-12 | 2021-10-12 | Crystal growth furnace suitable for Bridgman-Stockbarge method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1272145A (en) * | 1998-05-29 | 2000-11-01 | 东洋通信机株式会社 | Apparatus and method for manufacturing monocrystals, and monocrystal |
| CN1514046A (en) * | 2003-07-11 | 2004-07-21 | 中国科学院上海光学精密机械研究所 | Method for growing near-stoichiometric lithium niobate single crystal by using Bridgman method |
| JP2010120821A (en) * | 2008-11-20 | 2010-06-03 | Fuji Electric Holdings Co Ltd | Apparatus and method for growing crystal |
| CN204356436U (en) * | 2014-08-26 | 2015-05-27 | 江西匀晶光电技术有限公司 | The surplus material of a kind of crystal growing crucible is from bleeder |
-
2021
- 2021-10-12 CN CN202111187759.1A patent/CN113913918A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1272145A (en) * | 1998-05-29 | 2000-11-01 | 东洋通信机株式会社 | Apparatus and method for manufacturing monocrystals, and monocrystal |
| CN1514046A (en) * | 2003-07-11 | 2004-07-21 | 中国科学院上海光学精密机械研究所 | Method for growing near-stoichiometric lithium niobate single crystal by using Bridgman method |
| JP2010120821A (en) * | 2008-11-20 | 2010-06-03 | Fuji Electric Holdings Co Ltd | Apparatus and method for growing crystal |
| CN204356436U (en) * | 2014-08-26 | 2015-05-27 | 江西匀晶光电技术有限公司 | The surplus material of a kind of crystal growing crucible is from bleeder |
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