CN115613123A - Device and method for adding compound semiconductor material - Google Patents

Device and method for adding compound semiconductor material Download PDF

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Publication number
CN115613123A
CN115613123A CN202211186438.4A CN202211186438A CN115613123A CN 115613123 A CN115613123 A CN 115613123A CN 202211186438 A CN202211186438 A CN 202211186438A CN 115613123 A CN115613123 A CN 115613123A
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polycrystalline
capsule
crucible
frame
rod
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Chinese (zh)
Inventor
史艳磊
孙聂枫
徐成彦
秦敬凯
王书杰
邵会民
刘惠生
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CETC 13 Research Institute
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CETC 13 Research Institute
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Priority to CN202211186438.4A priority Critical patent/CN115613123A/en
Publication of CN115613123A publication Critical patent/CN115613123A/en
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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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • 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
    • 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
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • 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
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/42—Gallium arsenide
    • 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
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/44—Gallium phosphide

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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)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)

Abstract

A device and a method for adding compound semiconductor materials belong to the field of semiconductor crystal preparation. The device comprises a furnace body and a crucible, wherein a liftable annular feeding frame is arranged in the furnace body, an annular polycrystalline capsule frame is arranged on the feeding frame, and polycrystalline capsules with upper and lower openings are arranged on the polycrystalline capsule frame; the seed rod is connected with a driving motor, and a boss is arranged on the seed rod; the shape of the seed crystal rod and the shape of the central hole of the annular polycrystalline capsule rack are matched polygons; and the material releasing device is arranged on the upper edge of the crucible and is connected with a driving mechanism of the material releasing device. The method comprises the following steps: preparing materials, heating a crucible, and sequentially opening the plug of the polycrystalline capsule for adding the materials. The method adopts multi-step filling, the covering agent is placed in the crucible before the filling, and the polycrystalline material is added for multiple times after the covering agent is melted, so that the added polycrystalline material is submerged by the melted covering agent and is melted under the liquid level, and the loss of elements in the polycrystalline material is avoided.

Description

Device and method for adding compound semiconductor material
Technical Field
The invention belongs to the field of semiconductor crystal preparation, and relates to a device and a method for adding a compound semiconductor material before crystal growth.
Background
The compound semiconductor material has a high ionization pressure. For example, for indium phosphide, the ionization pressure is 2.75MPa in the vicinity of its melting point. In the process of growing a single crystal by the LEC method, a covering agent needs to be added into a crucible to ensure that a compound semiconductor material at a high temperature is in a covered state and the compound semiconductor material is not dissociated.
In the current single crystal growth method, when assembling the single crystal growth system, a compound semiconductor polycrystalline material and a covering agent (such as boron oxide) are first charged into a crucible, the charged polycrystalline material is basically in a block shape or a granular shape, during the heating process of melting the material, the covering agent is firstly melted because the melting point of the covering agent is lower than that of the polycrystalline material, the covering agent flows into the gaps of the polycrystalline material, the covering agent cannot completely cover the polycrystalline material, and when the polycrystalline material is completely melted, the covering agent completely covers the melt of the compound semiconductor because of the difference of density.
In the process of temperature rise, volatile elements (such as phosphorus in indium phosphide) in the polycrystalline material volatilize due to high temperature, so that the melt and the following crystals are not proportioned. For compound materials, the dissociation mainly occurs during the material melting, and the dissociated part is the part exposed outside the boron oxide.
The traditional method comprises the following steps: 1. by breaking the material into particles, it is ensured that when the material is filled, the gaps in the material are reduced; 2. the amount of the covering agent to be loaded is increased to cover the material as much as possible. However, the conventional method has many disadvantages: in the first method, the process of crushing the compound introduces impurities, which leads to the reduction of purity, and the influence of crushing on the degree of material compactness is limited; in the second method, by increasing the loading amount of the covering agent, on the one hand, the single use amount of the covering agent is increased, and on the other hand, an excessively thick covering agent causes difficulty in observation when crystals grow.
This problem becomes more severe as the crucible charge increases. For example, in the conventional LEC method for preparing indium phosphide, 1000g of boron oxide is added as a covering agent in a 10-inch crucible, the charging amount of indium phosphide polycrystal in the crucible is 20Kg, 100-200g of phosphorus element is lost in the heating and melting process of the material, 100-200g of phosphorus element is lost, the final 3-6Kg of material is in an unmatched state, and the influence on the yield of single crystal products is very large.
Therefore, there is a need for a method to reduce material loss at elevated temperatures of compounds.
Disclosure of Invention
The present invention has been made to solve the above problems.
The invention discloses a device for adding compound semiconductor material and a method for adding compound semiconductor material based on the device.
The device for adding the compound semiconductor material comprises a furnace body and a crucible in the furnace body, and is characterized in that: an annular feeding frame connected with a vertical lifting mechanism is arranged in the furnace body, an annular polycrystalline capsule frame is placed on the feeding frame, and 4-8 circular holes are uniformly formed in the annular polycrystalline capsule frame; a polycrystalline capsule with an upper opening and a lower opening is arranged in the round hole of the polycrystalline capsule rack; the seed rod is connected with a driving motor, and a boss is arranged on the seed rod; the seed rod penetrates through a central hole of the polycrystalline capsule rack, and the shape of the seed rod and the shape of the central hole of the annular polycrystalline capsule rack are matched polygons; the device also comprises a material releasing device arranged on the upper edge of the crucible, and the material releasing device is connected with a driving mechanism of the material releasing device.
Further, the material releasing device is a heating coil, and the diameter of the heating coil is matched with the size of the lower opening of the polycrystalline capsule.
Furthermore, a cover plate is arranged at the lower opening of the polycrystalline capsule, one end of the cover plate is connected with the lower end face of the polycrystalline capsule through a rotating shaft, and a shifting head is arranged at the opposite end of the cover plate; the material releasing device is a deflector rod.
A method for adding a compound semiconductor material is realized based on the device for adding the compound semiconductor material, and comprises the following steps:
step 1, plugging a lower opening of a polycrystalline capsule, and filling a polycrystalline material into the polycrystalline capsule;
step 2, placing the polycrystalline capsules into a capsule rack, placing the capsule rack on a feeding rack, mounting seed crystals on a seed crystal rod, and enabling the seed crystal rod to penetrate through a central hole of the polycrystalline capsule rack; connecting the feeding frame with a vertical lifting mechanism;
step 3, filling the covering agent or the covering agent and a small amount of polycrystalline material into a crucible, and filling the crucible into a furnace body;
step 4, sealing the furnace body, vacuumizing and filling inert gas;
step 5, heating the crucible to melt the materials in the crucible;
step 6, descending the feeding frame to enable the polycrystalline capsule frame to fall on a boss of the seed crystal rod; continuously descending the feeding frame to separate the feeding frame from the polycrystalline capsule frame;
step 7, starting a material releasing device to open an opening below the polycrystalline capsule, so that the polycrystalline material in the polycrystalline capsule falls into the crucible and is covered by the melt and the molten covering agent;
step 8, after the polycrystalline material in the crucible is completely melted, rotating the seed rod to drive the next polycrystalline capsule to be positioned above the material release device;
9, repeating the step 7 and the step 8 until all polycrystalline materials in the polycrystalline capsules fall into the crucible;
step 10, lifting a feeding frame, namely lifting the feeding frame, a polycrystalline capsule frame and a polycrystalline capsule to the top of a furnace body;
step 11, descending a seed crystal rod to enable the seed crystal to contact the melt and start crystal growth; and after the crystal growth is finished, cooling, deflating and disassembling the furnace.
The method is suitable for the compound semiconductor materials containing volatile elements, such as indium phosphide, gallium arsenide, gallium phosphide, zinc germanium phosphide, indium arsenide and the like.
Has the advantages that: the method adopts a multi-step filling mode, the covering agent is placed in the crucible before the filling, and the polycrystalline material is added for multiple times after the covering agent in the crucible is melted, so that the added polycrystalline material is submerged by the melted covering agent and is gradually melted under the liquid level, the loss of elements in the polycrystalline material is avoided, and the quality of crystals is improved.
Drawings
FIG. 1 is a schematic view of the structure of the device of the present invention,
fig. 2 is a schematic structural view of the feeding frame, including a front view and a top view,
fig. 3 is a schematic structural view of a polycrystalline capsule holder, including a front view and a top view,
FIG. 4 is a schematic sectional view of the seed shaft,
FIG. 5 is a schematic view of the assembly of the polycrystalline capsule, the polycrystalline capsule holder and the feeding holder,
FIG. 6 is a schematic structural view of an embodiment of a polycrystalline capsule,
figure 7 is a schematic view of the structure of a polycrystalline capsule holder cooperating with figure 6,
figure 8 is a state diagram of an embodiment of an apparatus,
figure 9 is a state diagram of another embodiment apparatus,
figure 10 is a diagram of the charging state of the device,
figure 11 is another charging state diagram of the device,
figure 12 is a state diagram of the device after the completion of the filling,
FIG. 13 is a view showing a state of the apparatus during crystal growth.
Wherein: the device comprises a furnace body 1, a crucible 2, a heater 2-1, a feeding frame 3, a polycrystalline capsule frame 4, a central hole 4-1, a positioning groove 4-2, a polycrystalline capsule 5, a shifting head 5-1, a rotating shaft 5-2, a cover plate 5-3, a positioning block 5-4, a vertical lifting mechanism 6, a seed rod 7, a boss 7-1, a driving motor 8, a heating coil 9, a shifting rod 10, a driving mechanism of a material releasing device 11, a rotating motor 12, a polycrystalline material 13, a covering agent 14, a covering agent melted by 15, seed crystals 16 and crystals 17.
Detailed Description
A device for adding compound semiconductor materials, referring to figure 1, comprises a furnace body 1 and a crucible 2 in the furnace body 1, wherein an annular feeding frame 3 connected with a vertical lifting mechanism 6 is arranged in the furnace body 1, an annular polycrystalline capsule frame 4 is arranged on the feeding frame 3, and 4-8 circular holes are uniformly formed in the annular polycrystalline capsule frame 4; a polycrystalline capsule 5 with an upper opening and a lower opening is arranged in a round hole of the polycrystalline capsule rack 4; the seed rod 7 is connected with a driving motor 8, and a boss 7-1 is arranged on the seed rod 7; the seed rod 7 passes through the central hole 4-1 of the polycrystalline capsule holder 4, and the shape of the seed rod 7 and the shape of the central hole 4-1 of the annular polycrystalline capsule holder 4 are matched polygons, as shown in fig. 3 and 4.
The structure of the annular feeding frame 3 is shown in fig. 2, the structure of the annular polycrystalline capsule frame 4 is shown in fig. 3, and the assembly of the polycrystalline capsules 5, the polycrystalline capsule frame 4 and the feeding frame 3 is shown in fig. 5.
The diameter of the lower opening of the polycrystalline capsule 5 is 1.5 to 2 times larger than the maximum block diameter of the polycrystalline material. The polycrystal material is filtered and screened by a screen with the diameter of 10-30mm, and according to the requirement, the diameter of the lower opening of the polycrystal capsule 5 is more than 45mm.
The capacity of the polycrystalline capsules 5 is related to the size of the crucible 2 and the number of polycrystalline capsules 5, and can be selected according to the requirements.
The apparatus further comprises a material release device arranged at the upper edge of the crucible 2, and the material release device is connected with a driving mechanism of the material release device.
The invention adds the polycrystal materials in the polycrystal capsules 5 into the crucible 2 in sequence, and the material release device realizes the function. The valve can be arranged below the polycrystalline capsule 5, the valve is closed during charging, and the valve is opened in sequence during charging, but the mode has a complex structure and is difficult to realize.
The invention provides two preferable schemes:
1. the material release device is a heating coil 9, and the diameter of the heating coil 9 is matched with the size of the lower opening of the polycrystalline capsule 5. In use, the lower opening of the polycrystalline capsule 5 is sealed with the covering agent 14, and when the polycrystalline capsule 5 needs to be filled, the heating coil 9 is used to heat the lower opening of the polycrystalline capsule 5, the covering agent 14 is melted, and the polycrystalline material 13 falls.
2. The material releasing device is a deflector rod 10, in order to match with the deflector rod 10, a cover plate 5-3 is arranged at the lower opening of the polycrystalline capsule 5, one end of the cover plate 5-3 is connected with the lower end face of the polycrystalline capsule 5 through a rotating shaft 5-2, and a deflector 5-1 is arranged at the opposite end of the cover plate 5-3, as shown in fig. 6. When the polycrystalline material dropping device is used, the deflector rod 10 is fixed, the polycrystalline capsule 5 is driven by the seed rod 7 to rotate, the deflector rod 10 is in contact with the deflector head 5-1, the cover plate 5-3 is pushed to rotate around the rotating shaft 5-2, the lower opening of the polycrystalline capsule 5 is opened, and the polycrystalline material 13 falls.
In the second scheme, a positioning block 5-4 is arranged on the outer side of the polycrystalline capsule 5, and the positioning block 5-4 and the shifting block 5-2 are arranged on the same side; the circular hole on the annular polycrystalline capsule holder 4 is provided with a positioning groove 4-2 matched with the positioning block 5-4, and the positioning groove 4-2 is arranged at the position closest to the outer edge of the annular polycrystalline capsule holder 4, as shown in fig. 6 and 7.
In fig. 6, the middle view is a bottom view of polycrystalline capsule 5, and the lower view is a bottom view of polycrystalline capsule 5 with the lower opening portion opened.
According to the scheme, the polycrystalline capsule 5 can be positioned, the rotating shaft 5-2 is arranged on the innermost side of the polycrystalline capsule frame 4, the shifting head 5-1 is arranged on the outermost side of the polycrystalline capsule frame 4, and the polycrystalline capsule frame is convenient to assemble on the premise of ensuring the position.
In this embodiment, the crucible 2 is connected to a rotating motor 12.
Based on the above device, the present invention also provides a method for adding a compound semiconductor material, comprising the steps of:
step 1, plugging a lower opening of the polycrystalline capsule 5, and filling a polycrystalline material 13 into the polycrystalline capsule 5.
Corresponding to different release device schemes, the embodiment provides two plugging methods:
1. the lower opening of the polycrystalline capsule 5 is sealed by using a covering agent 14, and the lower opening of the polycrystalline capsule 5 is sealed by using a cover plate 5-3.
Step 2, placing the polycrystalline capsules 5 into a capsule frame 4, placing the capsule frame 4 on a feeding frame 3, mounting seed crystals 16 on a seed crystal rod 7, and enabling the seed crystal rod 7 to penetrate through a central hole 4-1 of the polycrystalline capsule frame 4; the feeding frame 3 is connected with a vertical lifting mechanism 6.
The capsule frame 4 is arranged on the feeding frame 3, and the capsule frame and the feeding frame are not in fixed relation; the shape of the seed rod 7 and the shape of the central hole 4-1 of the annular polycrystalline capsule frame 4 are matched polygons, in the embodiment, the matching is hexagonal, the matching between the seed rod and the central hole is not required to be tight, the tolerance margin can be slightly larger, and the holes can be conveniently recognized. The purpose of shape matching is to enable the seed rod 7 to drive the polycrystalline capsule holder 4 to rotate.
At the moment, the feeding frame 3 is arranged above the boss 7-1 of the seed rod 7.
The projection position of the seed rod 7 is in the center of the crucible 2, the diameter of the feeding frame 3 and the capsule frame 4 are arranged according to the diameter of the crucible 2, and the lower opening of the polycrystalline capsule 5 is ensured to be completely in the range of the crucible 2 when the material is added.
And 3, filling the covering agent 14 or the covering agent 14 and a small amount of polycrystalline material 13 into the crucible 2, and filling the crucible 2 into the furnace body 1.
When filling the crucible 2, the present embodiment proposes two solutions:
1. placing only the covering agent 14 in the crucible 2; 2. a small amount of polycrystalline material 13 and a covering agent 14 are placed in the crucible 2.
In the scheme 1, the covering agent 14 has a low melting point and can be quickly melted, so that the material can be added; in case of the 2 nd solution, more space is provided under the liquid surface when both the polycrystalline material 13 and the covering agent 14 are melted. In option 2, polycrystalline mass 13 is placed under the covering agent 14 and is uniformly disposed. The term "small amount" as used herein means that the covering agent 14 is completely melted and is always submerged by the melted covering agent during the melting of the polycrystalline material 13, thereby causing no element loss.
In this embodiment, a small amount of polycrystalline material 13 and a covering agent 14 are charged into the crucible 2.
The above steps complete the assembly of the device as shown in fig. 1. Figure 1 employs a first material release device scheme.
And 4, sealing the furnace body 1, vacuumizing, and filling inert gas with specific pressure.
And step 5, heating the crucible 2 to melt the material in the crucible 2. In this embodiment, the covering agent 14 and the polycrystalline material 13 in the crucible 2 are melted one after the other to form a layered melt.
Step 6, descending the feeding frame 3 to enable the polycrystalline capsule frame 4 to fall on a boss 7-1 of the seed rod 7; the material feeding frame 3 is further lowered to separate the material feeding frame 3 from the polycrystalline capsule frame 4, as shown in fig. 8 and 9.
Fig. 8 employs a first material release arrangement and fig. 9 employs a second material release arrangement.
After the polycrystalline capsule holder 4 descends to the right position, in fig. 8, the heating coil 9 is close to the lower opening of the polycrystalline capsule 5, and in fig. 9, the horizontal position of the deflector rod 10 is the same as that of the deflector head 5-1.
The feeding frame 3 is separated from the polycrystalline capsule frame 4, and the aim is that the feeding frame 3 does not influence the rotation of the polycrystalline capsule frame 4.
Step 7, the material releasing device is started, so that the lower opening of the polycrystalline capsule 5 is opened, and the polycrystalline material 13 in the polycrystalline capsule 5 falls into the crucible 2 and is covered by the melt and the melted covering agent 15.
When the first material release device scheme is adopted, the seed rod 7 drives the polycrystalline capsule rack 4 to rotate, the polycrystalline capsules 5 are rotated above the heating coil 9, and the seed rod 7 stops rotating; the heating coil 9 is started, so that the covering agent 14 blocking the lower opening of the polycrystalline capsule 5 is melted, and the lower opening of the polycrystalline capsule 5 is opened.
When the second material release device scheme is adopted, the seed rod 7 drives the polycrystalline capsule 5 to rotate continuously, the deflector rod 10 is matched with the deflector head 5-1, the cover plate 5-3 is pushed to rotate around the rotating shaft 5-2, and the lower opening of the polycrystalline capsule 5 is opened. After the deflector rod 10 is separated from the deflector head 5-1, the seed rod 7 stops rotating.
The two material releasing devices gradually open the lower opening of the polycrystalline capsule 5, and polycrystalline material 13 in the polycrystalline capsule 5 slowly falls into the crucible 2.
The melt in the crucible 2 has two components: above is the molten covering agent 15 and below is the molten polycrystalline material. For compound semiconductor materials, the melt will be somewhat denser than the solid, and the polycrystalline material 13 will float on the polycrystalline melt after falling into the crucible 2. Such as an indium phosphide melt density of 5.05g/cm 3 The crystal density is 4.787 g/cm 3 . The density of the molten covering agent 15 is less than the density of the polycrystalline material 13, e.g. the density of liquid boron oxide is 2.460 g/cm 3 The melt in crucible 2 has two components: above is the molten covering agent 15 and below is the molten polycrystalline material. For compound semiconductor materials, the melt will be somewhat denser than the solid, and the polycrystalline material 13 will float on the polycrystalline melt after falling into the crucible 2. Such as an indium phosphide melt density of 5.05g/cm 3 The crystal density is 4.787 g/cm 3 . The density of the molten covering agent 15 is less than the density of the polycrystalline material 13, e.g. the density of liquid boron oxide is 2.460 g/cm 3 . Depending on the amount charged, the polycrystalline material 13 is partially immersed in the molten polycrystalline material and partially on top of the molten polycrystalline material, such as in the form of icebergs in water, as shown in FIG. 10.
In order to avoid the polycrystalline material 13 introduced into the crucible 2 from emitting molten covering agent 15, the invention proposes two measures, which can be carried out separately or simultaneously:
1. the loading amount of the polycrystalline material 13 in the polycrystalline capsule 5 increases in order of the charging.
At the initial stage of charging, the polycrystalline material 13 is less loaded in the polycrystalline capsules 5, so that it is submerged under the molten covering agent 15 after falling into the crucible 2. With the addition of the polycrystalline material 13, the melt in the crucible 2 is more and more, the melt depth is increased, and more space is provided for the polycrystalline material 13 to sink into the melt, so that the filling amount of the polycrystalline material 13 in the polycrystalline capsules 5 can be sequentially increased according to the material adding sequence, and the efficiency is improved.
2. During the fall of the polycrystalline material 13 in the polycrystalline capsules 5 into the crucible 2, the crucible 2 is rotated.
During the charging process, the crucible 2 can be kept rotating, achieving the above conditions.
If the polycrystalline capsule 5 and the crucible 2 do not move relatively, the polycrystalline material 13 in the polycrystalline capsule 5 may fall at the same position, and if the covering condition is satisfied, the amount of the polycrystalline material 13 to be charged may be decreased or the amount of the covering agent 14 to be used may be increased. By rotating the crucible 2, the polycrystalline material 13 is caused to fall relatively uniformly on one circumference of the crucible 2, overcoming the above-mentioned drawbacks.
The rotation speed of the crucible 2 is controlled in one filling period of the polycrystalline capsules 5, and the crucible 2 rotates at least once.
After the polycrystalline material 13 falls into the crucible 2, the polycrystalline material 13 may diffuse over the surface of the polycrystalline melt due to the presence of the polycrystalline melt and the rotation of the crucible 2, as shown in FIG. 11.
And 8, after the polycrystalline material 13 in the crucible 2 is completely melted, rotating the seed rod 7 to drive the next polycrystalline capsule 5 to be positioned above the material release device.
After a polycrystalline capsule 5 is completely filled, the filling is continued after the added polycrystalline material 13 is completely melted.
Step 9, repeating step 7 and step 8 until all the polycrystalline material 13 in the polycrystalline capsules 5 falls into the crucible 2.
Step 10, lifting the feeding frame 3, and lifting the feeding frame 3, the polycrystalline capsule frame 4 and the polycrystalline capsules 5 to the top of the furnace body 1, as shown in fig. 12.
The drive mechanism 11 of the material release device is activated to move the material release device away from the crystal growth to avoid affecting the crystal growth.
Step 11, descending the seed rod 7 to enable the seed crystal 16 to contact the melt, and starting to grow a crystal 17, as shown in figure 13; and after the crystal 17 is grown, cooling, deflating and disassembling the furnace.

Claims (10)

1. A device for adding compound semiconductor materials comprises a furnace body (1) and a crucible (2) in the furnace body (1), and is characterized in that an annular feeding frame (3) connected with a vertical lifting mechanism (6) is arranged in the furnace body (1), an annular polycrystalline capsule frame (4) is placed on the feeding frame (3), and 4-8 round holes are uniformly formed in the annular polycrystalline capsule frame (4); a polycrystalline capsule (5) with an upper opening and a lower opening is arranged in the round hole of the polycrystalline capsule rack (4); the seed rod (7) is connected with a driving motor (8), and a boss (7-1) is arranged on the seed rod (7); the seed rod (7) penetrates through a center hole (4-1) of the polycrystalline capsule frame (4), and the shape of the seed rod (7) and the shape of the center hole (4-1) of the annular polycrystalline capsule frame (4) are matched polygons;
the device also comprises a material releasing device arranged on the upper edge of the crucible (2), and the material releasing device is connected with a driving mechanism (11) of the material releasing device.
2. The device according to claim 1, wherein the material release means is a heating coil (9), the diameter of the heating coil (9) matching the size of the lower opening of the polycrystalline capsule (5).
3. The device according to claim 1, wherein the lower opening of the polycrystalline capsule (5) is provided with a cover plate (5-3), one end of the cover plate (5-3) is connected with the lower end face of the polycrystalline capsule (5) through a rotating shaft (5-2), and the opposite end of the cover plate (5-3) is provided with a shifting block (5-1); the material releasing device is a deflector rod (10).
4. The device according to claim 3, wherein a positioning block (5-4) is arranged on the outer side of the polycrystalline capsule (5), and the positioning block (5-4) is arranged on the same side with the shifting block (5-2); the circular hole on the annular polycrystalline capsule frame (4) is provided with a positioning groove (4-2) matched with the positioning block (5-4), and the positioning groove (4-2) is arranged at a position closest to the outer edge of the annular polycrystalline capsule frame (4).
5. The device according to claim 1, characterized in that the crucible (2) is connected to a rotating electrical machine (12).
6. A method for adding a compound semiconductor material, which is implemented based on the apparatus for adding a compound semiconductor material according to any one of claims 1 to 5, comprising the steps of:
step 1, plugging a lower opening of a polycrystalline capsule (5), and filling a polycrystalline material (13) into the polycrystalline capsule (5);
step 2, putting the polycrystalline capsules (5) into a capsule rack (4), putting the capsule rack (4) on a feeding rack (3), installing seed crystals (16) on a seed crystal rod (7), and enabling the seed crystal rod (7) to penetrate through a central hole (4-1) of the polycrystalline capsule rack (4); connecting the feeding frame (3) with a vertical lifting mechanism (6);
step 3, filling the covering agent (14) or the covering agent (14) and a small amount of polycrystalline material (13) into the crucible (2), and filling the crucible (2) into the furnace body (1);
step 4, sealing the furnace body (1), vacuumizing and filling inert gas;
step 5, heating the crucible (2) to melt the material in the crucible (2);
step 6, descending the feeding frame (3) to enable the polycrystalline capsule frame (4) to fall on a boss (7-1) of the seed rod (7); continuously descending the feeding frame (3) to separate the feeding frame (3) from the polycrystalline capsule frame (4);
step 7, starting a material releasing device, so that an opening below the polycrystalline capsule (5) is opened, and the polycrystalline material (13) in the polycrystalline capsule (5) falls into the crucible (2) and is covered by the melt and the melted covering agent (15);
step 8, after the polycrystalline material (13) in the crucible (2) is completely melted, rotating the seed rod (7) to drive the next polycrystalline capsule (5) to be positioned above the material release device;
9, repeating the step 7 and the step 8 until all polycrystalline materials (13) in the polycrystalline capsules (5) fall into the crucible (2);
step 10, lifting the feeding frame (3), and lifting the feeding frame (3), the polycrystalline capsule frame (4) and the polycrystalline capsule (5) to the top of the furnace body (1);
step 11, descending the seed crystal rod (7) to enable the seed crystal (16) to contact the melt and start the growth of the crystal (17); and after the crystal growth is finished, cooling, deflating and disassembling the furnace.
7. The method of claim 6,
in the step 1, a covering agent (14) is used for blocking the lower opening of the polycrystalline capsule (5); in the step 7, the heating coil (9) is started, so that the covering agent (14) for blocking the lower opening of the polycrystalline capsule (5) is melted, and the lower opening of the polycrystalline capsule (5) is opened.
8. The method of claim 6,
in the step 1, a cover plate (5-3) is used for blocking a lower opening of the polycrystalline capsule (5); in the step 7, the polycrystalline capsule (5) is driven to rotate through the seed rod (7), the deflector rod (10) is matched with the deflector head (5-1), the cover plate (5-3) rotates around the rotating shaft (5-2), and the lower opening of the polycrystalline capsule (5) is opened.
9. The method according to claim 6, wherein the loading of polycrystalline material (13) in the polycrystalline capsules (5) increases in sequence according to the order of charging.
10. Method according to claim 6, characterized in that the crucible (2) is rotated during the fall of the polycrystalline material (13) in the polycrystalline capsule (5) into the crucible (2).
CN202211186438.4A 2022-09-28 2022-09-28 Device and method for adding compound semiconductor material Pending CN115613123A (en)

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