CN218404506U - Centrifugal crystal growth device of compound semiconductor - Google Patents

Centrifugal crystal growth device of compound semiconductor Download PDF

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Publication number
CN218404506U
CN218404506U CN202222566845.XU CN202222566845U CN218404506U CN 218404506 U CN218404506 U CN 218404506U CN 202222566845 U CN202222566845 U CN 202222566845U CN 218404506 U CN218404506 U CN 218404506U
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centrifugal wheel
centrifugal
crucible
support rod
main shaft
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王书杰
孙聂枫
徐森锋
史艳磊
李晓岚
邵会民
刘峥
王阳
姜剑
康永
张鑫
谷伟侠
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CETC 13 Research Institute
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CETC 13 Research Institute
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Abstract

The device comprises a centrifugal motor, a rotating main shaft, a supporting rod fixed on the rotating main shaft, a centrifugal wheel connected with the supporting rod, a graphite crucible arranged on the inner side of the edge of the centrifugal wheel, a seed rod arranged on the rotating main shaft and driven by the seed rod, and magnetic field generators arranged on the upper side and the lower side of the centrifugal wheel. Adopt the utility model provides a device has accelerated the transmission of carbon atom, and the formation of inclusion and polycrystal can effectively be avoided in the continuous supply of growth interface department carbon atom, realizes the high-quality silicon carbide single crystal of high-efficient preparation low defect, nothing mix with.

Description

Centrifugal crystal growth device of compound semiconductor
Technical Field
The utility model belongs to semiconductor material preparation field relates to a compound semiconductor's centrifugal crystal growth device.
Background
Silicon carbide is an important new-generation compound semiconductor material, has an important role in the aspect of preparing high-power electronic devices, and is widely applied to the fields of aerospace, automobiles and the like.
The commonly used growth methods at present are: physical vapor deposition, melt processes, and the like. Physical vapor deposition has high energy consumption, low efficiency and higher dislocation density, and a melt method can prepare the silicon carbide single crystal with low dislocation, but because the saturated vapor pressure of the proportioned melt is extremely high, the realization is difficult, and only the growth of the melt under the non-proportioned degree can be carried out, so that the proportion of the melt at the growth interface is poor, and polycrystal and inclusion are easily formed.
The methods have the problems of high energy consumption, poor quality of grown crystals and the like because of poor melt proportioning, and are difficult to realize the high-efficiency preparation of low-defect and high-quality silicon carbide single crystals.
Disclosure of Invention
In order to overcome the defects of the prior art, the utility model is provided.
The utility model adopts the technical proposal that: a centrifugal crystal growth device for a compound semiconductor comprises a rotating main shaft connected with a centrifugal motor, a supporting rod fixed on the rotating main shaft, a centrifugal wheel connected with the supporting rod, a crucible groove arranged on the inner side of the edge of the centrifugal wheel, a ceramic support arranged in the crucible groove, a graphite crucible arranged in the ceramic support, a seed rod arranged on the rotating main shaft under the drive of the seed rod, and magnetic field generators arranged on the upper side and the lower side of the centrifugal wheel.
Furthermore, the magnetic field generators are provided with a plurality of groups, magnetic lines of force in opposite directions are sequentially generated, and the number of the magnetic field generators generating the forward magnetic lines of force and the reverse magnetic lines of force is the same.
Furthermore, the magnetic field generator is arranged on the inner side of the edge of the centrifugal wheel, and the action range of the magnetic force lines does not exceed the top of the graphite crucible.
The existing research shows that the supergravity is used as a reinforced separation means, so that the separation of elements in the alloy can be realized, and the purification of substances and the refinement of solidification structures of two alloys can be realized by using the means.
Yangyu thickness in the basic research on the refinement of the metal solidification structure and the element segregation behavior by the hypergravity, it is disclosed that the C separation in the Fe-C alloy is already performed under the condition that the hypergravity field G =70G, and the Fe-0.99wt% of C low-carbon steel austenite grains are significantly refined.
Centrifugal force is one means of creating supergravity.
The utility model discloses with polycrystalline silicon as for in the graphite crucible, the graphite crucible is arranged in the centrifugal hypergravity device that has invariable alternating magnetic field. After the centrifugal device is started, the graphite crucible generates induction current in a constant alternating magnetic field to heat, so that polycrystalline silicon is melted, meanwhile, part of graphite is dissolved into silicon melt to form silicon-carbon melt, and carbon atoms move towards the rotating main shaft under the action of centrifugal force. And seed crystals are arranged on the side of the rotating shaft, and because the seed crystals are close to the enriched carbon atoms, the seed crystals contact the silicon-carbon melt to prepare the silicon carbide single crystal.
Has the advantages that: adopt the utility model provides a device has accelerated the transmission of carbon atom, and the formation of inclusion and polycrystal can effectively be avoided in the continuous supply of growth interface department carbon atom. Compared with physical vapor deposition, the method has the advantages of small thermal stress of growth interface, small and symmetrical temperature gradient, and dislocation density of the prepared 2-6 inch silicon carbide can reach 100-5000cm -2 And the high-quality silicon carbide single crystal with low defect and no inclusion can be efficiently prepared.
Drawings
FIG. 1 is a schematic view of the structure of the device of the present invention,
figure 2 is a schematic view of the device after loading,
FIG. 3 is a schematic view showing the state of the apparatus during the crystal growth,
figure 4 is a schematic view of the cooling water circuit of the device,
FIG. 5 is a schematic diagram of a centrifugal wheel structure,
FIG. 6 is a schematic view of another direction of the centrifugal wheel.
Wherein: 1: a centrifugal wheel; 1-1: a crucible tank; 1-2: a support rod jack; 1-3: pressing blocks of the supporting rods; 1-4: mounting holes; 2: a ceramic support; 3: a graphite crucible; 4: a reverse magnetic line of force; 5: a forward magnetic line of force; 6: covering the crucible; 7: seed crystals; 8: a crystal; 9: melting the materials; 10: a seed rod; 11: driving a seed crystal rod; 12: rotating the main shaft; 13: a magnetic field generator; 14: a centrifugal motor; 15: a support bar; 15-1: a cooling water pipe; 15-2: a support rod plug; 15-3: a circulating water pipe; 16: a shielding layer; 17: a heat-insulating layer; 18: polycrystalline silicon.
Detailed Description
A centrifugal crystal growth device of a compound semiconductor, referring to fig. 1-2, comprises a centrifugal motor 14, a rotating main shaft 12 connected with the centrifugal motor 14, a support rod 15 fixed on the rotating main shaft 12, a centrifugal wheel 1 connected with the support rod 15 through a support rod jack 1-2, a crucible groove 1-1 arranged on the inner side of the edge of the centrifugal wheel 1, a ceramic support 2 arranged in the crucible groove 1-1, a graphite crucible 3 arranged in the ceramic support 2, a seed rod 10 arranged on the rotating main shaft 12 through a seed rod drive 11 and aligned with the graphite crucible 3, and magnetic field generators 13 arranged on the upper side and the lower side of the centrifugal wheel 1.
The inner side of the edge of the centrifugal wheel 1 is provided with a crucible groove 1-1, a ceramic support 2 is arranged in the crucible groove 1-1, and the shape of the ceramic support 2 is matched with that of the crucible groove 1-1, as shown in figure 5.
In the embodiment, the rotating main shaft 12 is divided into two parts, the lower part mainly plays a role in supporting and rotating, the top of the rotating main shaft 12 is provided with a circulating water pipe 15-3, the circulating water pipe 15-3 is communicated with a cooling water pipe 15-1, and the cooling water pipe 15-1 is provided with an opening at the outer side of the centrifugal wheel 1.
In operation, the graphite crucible 3 is arranged in the ceramic holder 2. The top of the graphite crucible 3 is provided with a crucible sealing cover 6, and the center of the crucible sealing cover 6 is opened. The lid 6 prevents the outflow of material during operation, and the central opening allows the seed crystal 7 to penetrate into the graphite crucible 3.
The seed rod 10 points to the center of the central opening of the crucible cover 6.
The magnetic field generators 13 are provided with a plurality of groups, and sequentially generate magnetic lines of force in opposite directions, and the number of the magnetic field generators generating the forward magnetic lines of force is the same as that of the magnetic field generators generating the reverse magnetic lines of force.
The magnetic field generator 13 is arranged at the inner side of the edge of the centrifugal wheel 1, and the generated magnetic lines of force do not intersect with the centrifugal wheel 1, so that the centrifugal wheel 1 is prevented from generating high temperature, and the action range of the magnetic lines of force does not exceed the top of the graphite crucible 3.
The part of the support rod 15 in the range covered by the magnetic field generator 13 is provided with a shielding layer 16 and a heat insulation layer 17, so that the support rod 15 is prevented from generating high temperature.
In this embodiment, the seed rod 10 intersects the circulating water pipe 15-3 and passes through the circulating water pipe 15-3, and the cooling water passing through the circulating water pipe 15-3 can act on the seed rod 10. The seed rod 10 is provided with a rubber ring at a position penetrating through the rotating main shaft 12 to prevent water leakage.
Referring to fig. 6, a support rod pressing block 1-3 is arranged on a support rod insertion hole 1-2 of the centrifugal wheel 1 and is connected to the centrifugal wheel 1 through a mounting hole 1-4 which extends into the centrifugal wheel 1.
The height of the inner part of the ceramic support 2 is more than 1/2 of the height of the graphite crucible 3, namely, the ceramic support 2 can wrap at least half of the graphite crucible 3.
If temperature measurement is needed, a temperature measuring device can be arranged on the seed crystal rod, and a temperature measuring conducting wire can be led out through 15-3 without being influenced by rotation of the device.
In order to improve the efficiency, 2 graphite crucibles 3 can be symmetrically arranged on the inner side of the edge of the centrifugal wheel 1.
The structure and the function of each part of the present invention will be further explained by the using steps of the device.
When the silicon carbide crystal is prepared by using the utility model, the method comprises the following steps:
step 1, placing polycrystalline silicon 18 in a graphite crucible 3, and assembling a crucible cover 6 on a port of the graphite crucible 3; placing a ceramic support 2 in the crucible groove 1-1, and placing a graphite crucible 3 in the ceramic support 2; assembling a seed crystal 7 on a seed crystal rod 10; the centrifugal wheel 1 is connected to a support rod 15 and fixed to the rotary spindle 12.
When the centrifugal wheel 1 is connected with the supporting rod 15, firstly, the supporting rod pressing block 1-3 is moved away, the supporting rod plug 15-2 integrated with the supporting rod 15 is placed in the supporting rod insertion hole 1-2, then, the supporting rod pressing block 1-3 is reset, and the supporting rod pressing block is connected to the centrifugal wheel 1 through the mounting hole 1-4 by using a bolt.
The assembled device is shown in fig. 2.
Because the centrifugal wheel 1 is in a high-speed rotation state during working, two groups of support rod pressing blocks 1-3 are symmetrically arranged on the centrifugal wheel 1.
And 2, starting a plurality of groups of magnetic field generators 13 to form alternate reverse magnetic lines 4 and forward magnetic lines 5 on the inner side of the centrifugal wheel 1.
And 3, injecting water into the cooling water pipe 15-1 through a circulating water pipe 15-3.
The utility model discloses in, the device does not need airtight space at the during operation, and the cooling water flows through cooling water pipe 15-1.
And 4, starting a centrifugal motor 14 to rotate the whole system, generating induction current in the alternating reverse magnetic lines 4 and forward magnetic lines 5 of force by the graphite crucible 3 to heat, melting the polycrystalline silicon 18, dissolving part of graphite into the silicon melt to form a silicon-carbon melt 9, and moving carbon atoms to the side of the rotating main shaft 12 under the action of centrifugal force.
The crucible cover 6 can hold the melt 9 in the graphite crucible 3.
The magnetic field generator 13 is arranged at the inner side of the edge of the centrifugal wheel 1, the generated magnetic force line does not intersect with the centrifugal wheel 1, and the centrifugal wheel 1 does not cut the magnetic force line to generate high temperature.
The part of the support rod 15 in the range covered by the magnetic field generator 13 is provided with a shielding layer 16 and a heat insulation layer 17, so that the support rod 15 is prevented from generating high temperature.
Because the ceramic support 2 is arranged, the graphite crucible 3 is arranged in the ceramic support 2, the graphite crucible 3 has a certain distance with the centrifugal wheel 1, the graphite crucible 3 can cut magnetic lines, and the centrifugal wheel 1 does not cut the magnetic lines.
In the present embodiment, the magnetic field generator 13 covers a range from the bottom of the graphite crucible 3 to an intermediate position of the graphite crucible 3.
In this embodiment, the graphite crucible 3 has two functions: 1. and 2, providing carbon element for preparing the crystal.
In order to ensure the supply of carbon, the graphite crucible 3 has certain quality requirements: after the polycrystalline silicon 18 in the graphite crucible 3 is melted, the mass of the portion in contact with the graphite crucible 3 at the start of rotation is Mc, the mass of the polycrystalline silicon 18 is Ms, and the mass ratio of the two is: mc > 7.
The portion of the graphite crucible 3 that comes into contact with the beginning of rotation includes the bottom of the graphite crucible 3 and the side wall near the bottom. Since the crystal growth starts from the melt level and the consumption of the lower portion of the graphite crucible 3 is large, in this embodiment, the bottom thickness of the graphite crucible 3 is larger than the side wall thickness.
For greater safety, the height of the ceramic holder 2 is higher than the liquid level of the melt 9 in the graphite crucible 3, and the height of the inner part of the ceramic holder 2 is more than 1/2 of the height of the graphite crucible 3 to meet the requirement.
And 5, driving 11 through the seed crystal rod to enable the seed crystal to contact the melt 9, and increasing the concentration of carbon atoms because the carbon atoms raise the crystallization point of the melt 9, thereby realizing the growth of the silicon carbide single crystal at the contact interface of the seed crystal and the melt 9.
The density of carbon is less than the density of silicon. After the silicon-carbon melt 9 is formed, the silicon element with higher density moves to the graphite crucible 3 due to the action of centrifugal force, and the carbon element with lower density moves to the direction of the main rotating shaft 12, so that the density of carbon atoms on the surface of the melt 9 is increased.
In this embodiment, the rotation speed of the centrifugal motor 14 reaches a centrifugal force G greater than 300G.
The centrifugal force G is usually expressed in multiples of G (gravitational acceleration), and the conversion formula between G and the rotation speed is as follows:
G=1.11×10 -5 ×R×ω 2 xg, G centrifugal force, ω rotational speed in rmp, R radius in cm.
In this embodiment, the radius R can be regarded as the distance from the graphite crucible 3 to the rotation main shaft 12.
By the above formula, the rotation speed of the centrifugal rotating electric machine 14 can be calculated.
Experiments have shown that centrifugal forces G greater than 50G can cause separation of elements in the melt. In order to increase the separation speed of elements and further increase the synthesis speed, G is set to be larger than 300G in the embodiment.
In this example, the temperature of the silicon melt is between 1500 ℃ and 2200 ℃.
The carbon atoms are continuously supplied at the interface, the formation of inclusions and polycrystal can be effectively avoided, the thermal stress is small, the temperature gradient is small and symmetrical relative to the physical vapor deposition method, and the dislocation density of the prepared 2-6 inch silicon carbide can reach 100-5000cm -2

Claims (9)

1. The device is characterized by comprising a rotating main shaft (12) connected with a centrifugal motor (14), a supporting rod (15) fixed on the rotating main shaft (12), a centrifugal wheel (1) connected with the supporting rod (15), a crucible groove (1-1) arranged on the inner side of the edge of the centrifugal wheel (1), a ceramic support (2) arranged in the crucible groove (1-1), a graphite crucible (3) arranged in the ceramic support (2), a seed rod (10) arranged on the rotating main shaft (12) through a seed rod drive (11), and magnetic field generators (13) arranged on the upper side and the lower side of the centrifugal wheel (1).
2. The device according to claim 1, characterized in that a support rod insertion hole (1-2) is arranged in the middle of the centrifugal wheel (1), a removable support rod pressing block (1-3) is arranged above the support rod insertion hole (1-2), through mounting holes (1-4) are arranged on two sides of the support rod pressing block (1-3), the mounting holes (1-4) are arranged at positions corresponding to the centrifugal wheel (1), and support rod plugs (15-2) at two ends of the support rod (15) are connected with the centrifugal wheel (1) of the support rod (15) through the support rod insertion hole (1-2).
3. The apparatus according to claim 1, characterized in that the graphite crucible (3) is provided with a crucible cover (6) on top, the crucible cover (6) is provided with a central opening, and the seed rod (10) points to the center of the central opening of the crucible cover (6).
4. The device according to claim 1, wherein the magnetic field generators (13) are arranged in multiple groups, and sequentially generate magnetic lines in opposite directions, and the number of the magnetic field generators (13) generating the forward magnetic lines and the reverse magnetic lines is the same.
5. The device according to claim 1, characterized in that the magnetic field generator (13) is arranged inside the edge of the centrifugal wheel (1), and the action range of the magnetic force lines does not exceed the top of the graphite crucible (3).
6. A device according to claim 5, characterized in that the supporting rods (15) are provided with a shielding layer (16) and an insulating layer (17) at the parts within the coverage of the magnetic field generator (13).
7. The device according to claim 1, characterized in that a circulating water pipe (15-3) is arranged at the top of the rotating main shaft (12), the circulating water pipe (15-3) is communicated with a cooling water pipe (15-1), the cooling water pipe (15-1) is provided with an opening at the outer side of the centrifugal wheel (1), and the seed rod (10) penetrates through the circulating water pipe (15-3).
8. The device according to claim 1, the height inside the ceramic tray (2) being greater than 1/2 of the height of the graphite crucible (3).
9. The device according to any one of claims 1 to 8, characterized in that the graphite crucibles (3) are symmetrically arranged 2 inside the edge of the centrifugal wheel (1).
CN202222566845.XU 2022-09-28 2022-09-28 Centrifugal crystal growth device of compound semiconductor Active CN218404506U (en)

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Application Number Priority Date Filing Date Title
CN202222566845.XU CN218404506U (en) 2022-09-28 2022-09-28 Centrifugal crystal growth device of compound semiconductor

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Application Number Priority Date Filing Date Title
CN202222566845.XU CN218404506U (en) 2022-09-28 2022-09-28 Centrifugal crystal growth device of compound semiconductor

Publications (1)

Publication Number Publication Date
CN218404506U true CN218404506U (en) 2023-01-31

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