CN118207628A - Gallium arsenide monocrystal growing device and preparation method - Google Patents
Gallium arsenide monocrystal growing device and preparation method Download PDFInfo
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- CN118207628A CN118207628A CN202410627086.4A CN202410627086A CN118207628A CN 118207628 A CN118207628 A CN 118207628A CN 202410627086 A CN202410627086 A CN 202410627086A CN 118207628 A CN118207628 A CN 118207628A
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- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910001218 Gallium arsenide Inorganic materials 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002826 coolant Substances 0.000 claims abstract description 163
- 238000010438 heat treatment Methods 0.000 claims abstract description 82
- 239000013078 crystal Substances 0.000 claims abstract description 52
- 239000002994 raw material Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims description 28
- 229910052751 metal Inorganic materials 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 21
- 238000005452 bending Methods 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 238000000137 annealing Methods 0.000 claims description 7
- 230000007704 transition Effects 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 230000007423 decrease Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 9
- 238000002425 crystallisation Methods 0.000 abstract description 7
- 230000008025 crystallization Effects 0.000 abstract description 7
- 238000001816 cooling Methods 0.000 description 9
- 238000013003 hot bending Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 description 1
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 dislocation Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a gallium arsenide monocrystal growth device and a preparation method thereof, comprising a furnace body and a raw material containing device for containing raw materials, wherein the furnace body is arranged on a lifting driving device, a heating cavity is arranged in the furnace body, the lower end of the heating cavity is open, a heating part is arranged on the inner wall of the furnace body, a plurality of cooling medium rings arranged along the vertical direction are arranged in the heating cavity, the cooling medium cavities are arranged in the cooling medium rings, and a cooling medium inlet pipe and a cooling medium outlet pipe which are communicated with the cooling medium cavities are connected to the cooling medium rings. In the invention, only the flow rate of the cooling medium in each cooling medium ring is controlled, so that the temperature of different position areas in the heating cavity can be adjusted, and a required temperature gradient can be formed in the heating cavity, thereby ensuring the crystallization quality of the gallium arsenide single crystal and reducing the defect of the gallium arsenide single crystal.
Description
Technical Field
The invention relates to the technical field of gallium arsenide preparation, in particular to a gallium arsenide monocrystal growth device and a preparation method.
Background
Gallium arsenide (GaAs) single crystal growth is an important process in the semiconductor industry, primarily for the manufacture of high performance electronic and optoelectronic devices such as lasers, high speed integrated circuits, solar cells, and the like.
The Bridgman method, also called zone melting method or zone purification method, is a crystal growth technology invented by American physicist Percy Williams Bridgman, and is a common method for preparing gallium arsenide monocrystal at present.
The basic operation of the Bridgman method is as follows, first the pretreated feedstock is charged into a refractory crucible (typically a graphite, quartz or boron nitride crucible); the crucible is placed in a vacuum container, and the vacuum container is vacuumized; the vacuum vessel with the crucible is then placed in a heating furnace with precise temperature control, the heating furnace being provided with a temperature gradient; melting raw materials in the crucible by a heating furnace to form a melting zone; the temperature in the heating furnace is set in a range slightly higher than the melting point of the raw materials; then, as the crucible slowly moves downwards, the bottom of the crucible firstly enters a lower temperature area, so that the molten raw material starts to crystallize; starting from seed crystal, along with further lowering of crucible, the crystal is grown continuously and prolonged, and finally gallium arsenide monocrystal is obtained.
Wherein, the control of the temperature gradient in the heating furnace directly influences the crystallization quality of gallium arsenide. Defects in the crystal, such as dislocation, impurity stripes and the like, can cause the defects of dislocation, impurity stripes and the like in the crystal to influence the quality of the gallium arsenide single crystal if the temperature gradient is controlled improperly.
In the prior art, the temperature gradient in the heating furnace is difficult to accurately control, so that the gallium arsenide monocrystal product is easy to generate defects, and the quality of the product is not improved.
Disclosure of Invention
The invention aims to solve the problem that the gallium arsenide single crystal product is easy to generate defects due to the fact that the temperature gradient in a heating furnace is difficult to accurately control effectively in the prior art, and provides a gallium arsenide single crystal growth device and a preparation method, which can effectively solve the problem.
The invention aims at realizing the following technical scheme: the gallium arsenide monocrystal growing device comprises a furnace body and a raw material accommodating device for accommodating raw materials, wherein the furnace body is arranged on a lifting driving device, a heating cavity is arranged in the furnace body, the lower end of the heating cavity is open, a heating part is arranged on the inner wall of the furnace body, a plurality of cooling medium rings arranged along the vertical direction are arranged in the heating cavity, a cooling medium cavity is arranged in the cooling medium ring, and a cooling medium inlet pipe and a cooling medium discharge pipe which are communicated with the cooling medium cavity are connected to the cooling medium ring;
When the cooling medium is introduced into the cooling medium ring, the cooling medium exchanges heat with the area around the cooling medium ring to regulate the temperature of the area around the cooling medium ring.
Preferably, the cooling medium ring is positionally adjustable in the vertical direction; the cooling medium inlet pipe and the cooling medium outlet pipe pass through the upper end of the furnace body. The upper ends of the cooling medium inlet pipe and the cooling medium outlet pipe extend out of the upper end of the furnace body, and an operator can adjust the height position of the cooling medium ring by lifting the upper ends of the cooling medium inlet pipe and the cooling medium outlet pipe, so that the cooling medium ring moves to the required height position.
Preferably, the lower end of the cooling medium inlet pipe is connected with the inner side of the cooling medium ring through a transition pipe, and the lower end of the cooling medium outlet pipe is connected with the inner side of the cooling medium ring through a transition pipe.
Preferably, the upper end of the furnace body is provided with a through hole through which a cooling medium inlet pipe or a cooling medium outlet pipe can pass, the periphery of the through hole is provided with a mounting groove, and a clamping piece is arranged in the mounting groove; the clamping piece comprises a fixed ring and a plurality of thermal bending pieces, the fixed ring is fixedly arranged in the mounting groove, one end of each thermal bending piece is connected with the fixed ring, and the other end of each thermal bending piece is provided with a contact part; the thermal bending piece is arranged in a circular array and consists of a first metal layer and a second metal layer, the first metal layer is positioned on the outer side of the second metal layer, and the thermal expansion coefficient of the first metal layer is larger than that of the second metal layer; a cooling medium inlet pipe or a cooling medium outlet pipe passes through the space between the hot bent sheets on the clamping piece; when the temperature of the hot bent piece increases, the end of the hot bent piece provided with the contact part bends towards the center direction of the cooling medium inlet pipe or the cooling medium outlet pipe.
Preferably, the cooling medium is one of nitrogen, argon and carbon dioxide.
Preferably, the heating component is a heating wire, and the heating wires are arranged in a spiral shape.
Preferably, the raw material containing device comprises a crucible, a vacuum container body and a vacuum container cover, wherein the raw material is placed in the crucible, the crucible is placed in the vacuum container body, the vacuum container cover is connected to the upper end of the vacuum container body in a sealing way, and the interior of the vacuum container body is vacuumized.
Preferably, the crucible is a boron nitride crucible or a quartz crucible.
A preparation method of gallium arsenide single crystal comprises the following specific steps:
firstly, placing raw materials into a crucible, then placing the crucible into a vacuum container main body, mounting a vacuum container cover at the upper end of the vacuum container main body, and then vacuumizing the vacuum container main body;
Step two, placing a raw material accommodating device filled with raw materials below the furnace body, driving the furnace body to descend to a heating initial position through a lifting driving device, and completely positioning the raw material accommodating device in a heating cavity in the furnace body at the moment;
Starting a heating part, introducing cooling medium into the cooling medium rings through cooling medium inlet pipes, and regulating the inlet speed of the cooling medium in each cooling medium ring to enable the inner sides of the cooling medium rings to form different temperature areas, so that a temperature gradient is formed in a heating cavity, and the temperature in the heating cavity gradually decreases from top to bottom; the upper end part of the heating cavity is a melting heating area, and the raw materials are placed in the melting heating area; heating the temperature in the melting heating zone to 1238 ℃ and above to melt the feedstock;
Step three, driving the furnace body to ascend through the lifting driving device, and finishing the growth of gallium arsenide monocrystal after the raw materials undergo a shouldering process, an isodiametric process and an annealing process.
Preferably, the moving speed in the shoulder placing process is 1-2mm/h; the moving speed in the constant diameter process is 2-4mm/h.
The beneficial effects of the invention are as follows:
1. In the invention, only the flow rate of the cooling medium in each cooling medium ring is controlled, so that the temperature of different position areas in the heating cavity can be adjusted, and a required temperature gradient can be formed in the heating cavity, thereby ensuring the crystallization quality of the gallium arsenide single crystal and reducing the defect of the gallium arsenide single crystal.
2. When the gallium arsenide monocrystal is prepared, the furnace body moves but the raw materials do not move, so that the phenomenon that the crystal is disturbed in the growth and crystallization process of gallium arsenide to influence the final crystallization quality can be effectively avoided.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a schematic structural view of the temperature adjusting unit.
Fig. 3 is an enlarged view of a portion a in fig. 1.
Fig. 4 is a schematic structural view of the clamping member.
1. The device comprises a lifting driving device 2, a vacuum container main body 3, a vacuum container cover, a crucible 4, a crucible 5, seed crystals 6, raw materials 7, a furnace body 8, a heating component 9, a temperature adjusting unit 91, a cooling medium ring 92, a cooling medium cavity 93, a cooling medium inlet pipe 94, a cooling medium discharge pipe 95, a transition pipe 10, a mounting groove 11, a fixing ring 12, a hot bending piece 121, a first metal layer 122, a second metal layer 13 and a contact component.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which are derived by a person skilled in the art based on the embodiments of the invention, fall within the scope of protection of the invention.
It will be appreciated by those skilled in the art that in the present disclosure, the terms "longitudinal," "transverse," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," etc. refer to an orientation or positional relationship based on that shown in the drawings, which is merely for convenience of description and to simplify the description, and do not indicate or imply that the apparatus or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore the above terms should not be construed as limiting the present invention.
It will be understood that the terms "a" and "an" should be interpreted as referring to "at least one" or "one or more," i.e., in one embodiment, the number of elements may be one, while in another embodiment, the number of elements may be plural, and the term "a" should not be interpreted as limiting the number.
As shown in fig. 1 to 4, a gallium arsenide single crystal growing device comprises a furnace body 7 and a raw material accommodating device for accommodating raw materials 6, wherein the furnace body 7 is arranged on a lifting driving device 1, a heating cavity is arranged in the furnace body 7, the lower end of the heating cavity is open, a heating part 8 is arranged on the inner wall of the furnace body 7, a plurality of cooling medium rings 91 arranged along the vertical direction are arranged in the heating cavity, a cooling medium cavity 92 is arranged in the cooling medium rings 91, and a cooling medium inlet pipe 93 and a cooling medium outlet pipe 94 which are communicated with the cooling medium cavity 92 are connected to the cooling medium rings 91; when the cooling medium is introduced into the cooling medium ring 91, the cooling medium exchanges heat with the area around the cooling medium ring 91 to adjust the temperature of the area around the cooling medium ring 91.
In the invention, the furnace body 7 is of a cylindrical structure with an open lower end and a closed upper end, and the furnace body 7 is driven to move along the vertical direction by the lifting driving device 1. The heating part 8 in the heating cavity is used for heating the furnace body 7, and the cooling medium is introduced into the cooling medium cavity 92 in the cooling medium ring 91 through the cooling medium inlet pipe 93 and then discharged through the cooling medium discharge pipe 94; the cooling medium in the cooling medium chamber 92 will exchange heat with the area around the cooling medium ring 91, and as the temperature of the cooling medium itself is far lower than the temperature in the heating chamber, the cooling medium will absorb heat from the surrounding area and take heat out from the cooling, thereby lowering the temperature of the surrounding area of the cooling medium ring 91; and the greater the flow rate of the cooling medium, the more heat the cooling medium brings out per unit time, and thus the greater the temperature drop in the area around the cooling medium ring 91; conversely, if the flow velocity of the cooling medium is smaller and the amount of heat carried out by the cooling medium per unit time is smaller, the temperature drop in the area around the cooling medium ring 91 is smaller; in actual operation, only the flow rate of the cooling medium flowing into each cooling medium ring 91 needs to be controlled, so that the temperature drop of the area around the cooling medium ring 91 can be controlled, and further different temperature areas are formed near different cooling medium rings 91, so that a temperature gradient is formed in the vertical direction of the heating cavity. The cooling medium ring 91 gradually increases the inflow flow rate of the cooling medium from top to bottom, so that the temperature in the heating chamber gradually decreases from top to bottom.
The number of the coolant loops 91 and the arrangement density may be determined according to actual needs.
Wherein the cooling medium rings 91 are position-adjustable in the vertical direction, and the distance between two adjacent cooling medium rings 91 can be adjusted by adjusting the position of the cooling medium rings 91 in the vertical direction. The cooling medium inlet pipe 93 and the cooling medium outlet pipe 94 pass through the upper end of the furnace body 7. Wherein, the upper end of the furnace body 7 is provided with a through hole which can lead the cooling medium inlet pipe 93 or the cooling medium outlet pipe 94 to pass through, the periphery of the through hole is provided with a mounting groove 10, and a clamping piece is arranged in the mounting groove 10; the clamping piece comprises a fixed ring 11 and a plurality of thermal bending pieces 12, wherein the fixed ring 11 is fixedly arranged in the mounting groove 10, one end of the thermal bending piece 12 is connected with the fixed ring 11, and the other end of the thermal bending piece 12 is provided with a contact part 13; the thermal bending pieces 12 are arranged in a circular array, the thermal bending pieces 12 are composed of a first metal layer 121 and a second metal layer 122, the first metal layer 121 is located on the outer side of the second metal layer 122, and the thermal expansion coefficient of the first metal layer 121 is larger than that of the second metal layer 122. A cooling medium inlet pipe 93 or a cooling medium outlet pipe 94 passes between the hot bent pieces 12 on the clamping member; when the temperature of the thermal bend 12 increases, the end of the thermal bend 12 on which the contact member 13 is provided is bent toward the center of the cooling medium inlet pipe 93 or the cooling medium outlet pipe 94.
When the furnace body 7 is not in a heating state, the temperature of the furnace body 7 is consistent with the room temperature, the temperature of the clamping piece is consistent with the room temperature, the contact part 13 on the hot bending piece 12 is contacted with the cooling medium inlet pipe 93 or the cooling pipe medium discharge pipe, the bending amplitude of the hot bending piece 12 is smaller, the contact pressure between the contact part 13 and the outer surface of the cooling medium inlet pipe 93 or the cooling pipe medium discharge pipe is smaller, the clamping force of the clamping piece on the cooling medium inlet pipe 93 or the cooling medium discharge pipe 94 is smaller, when an operator needs to adjust the cooling medium ring 91 up and down, the operator can easily overcome the friction force between the contact part 13 and the cooling medium inlet pipe 93 or the cooling pipe medium discharge pipe to enable the cooling medium inlet pipe 93 or the cooling pipe medium discharge pipe to move up and down, and when no external force is applied to the cooling medium inlet pipe 93 or the cooling pipe medium discharge pipe, the cooling medium inlet pipe 93 or the cooling pipe medium discharge pipe can stay at the current position stably under the clamping force of the clamping piece; when the furnace body 7 is in a heating state, the temperature of the furnace body 7 is greatly increased, the temperature of the clamping member is increased, and when the temperature of the hot bending piece 12 is increased, one end of the hot bending piece 12 provided with the contact part 13 is bent towards the center direction of the cooling medium inlet pipe 93 or the cooling medium outlet pipe 94, so that the pressure of the contact part 13 to the cooling medium inlet pipe 93 or the cooling medium outlet pipe 94 is increased, the clamping force of the clamping member to the cooling medium inlet pipe 93 or the cooling medium outlet pipe 94 is increased, and the cooling medium ring 91 can be firmly fixed at the current position, and the cooling medium ring 91 cannot be accidentally moved.
The lower end of the cooling medium inlet pipe 93 is connected to the inner side of the cooling medium ring 91 through a transition pipe 95, and the lower end of the cooling medium outlet pipe 94 is connected to the inner side of the cooling medium ring 91 through a transition pipe 95.
The cooling medium can be a gas medium or a liquid medium, and can be selected according to actual needs. In some embodiments of the present invention, the cooling medium is one of nitrogen, argon, and carbon dioxide.
The heating part 8 is an electric heating wire which is arranged in a spiral shape. The electric heating wire is closely attached to the inner wall of the furnace body 7. The two ends of the heating wire are respectively connected with a power supply, and the heating function is realized after the heating wire is electrified.
The raw material containing device comprises a crucible 4, a vacuum container main body 2 and a vacuum container cover 3, wherein raw materials 6 are placed in the crucible 4, the crucible 4 is placed in the vacuum container main body 2, the vacuum container cover 3 is connected to the upper end of the vacuum container main body 2 in a sealing way, and the interior of the vacuum container main body 2 is vacuumized.
Wherein the crucible 4 is made of a high temperature resistant material and has good heat resistance. In some embodiments of the present invention, the crucible 4 is a boron nitride crucible 4 or a quartz crucible 4. Both the boron nitride crucible 4 and the quartz crucible 4 have good stability and high temperature resistance, and do not react with the raw material 6 itself.
The vacuum vessel main body 2 and the vacuum vessel cover 3 are both made of quartz material.
A preparation method of gallium arsenide single crystal comprises the following specific steps:
Step one, putting a raw material 6 into a crucible 4, then putting the crucible 4 into a vacuum container body 2, mounting a vacuum container cover 3 at the upper end of the vacuum container body 2, and then vacuumizing the vacuum container body 2. Wherein the raw materials are gallium metal, arsenic source compound and mixture, the arsenic source compound can be selected from arsenic trioxide or arsine, and a seed crystal 5 is placed at the bottom of the crucible. The seed crystal 5 is a gallium arsenide crystal with high purity. The vacuum degree in the vacuum vessel main body 2 should be 0.001 Pa to 0.01 Pa.
Step two, placing a raw material containing device filled with raw materials 6 below the furnace body 7, driving the furnace body 7 to descend to a heating initial position through the lifting driving device 1, wherein the raw material containing device is completely positioned in a heating cavity in the furnace body 7;
Starting the heating part 8, introducing cooling medium into the cooling medium rings 91 through the cooling medium inlet pipes 93, and regulating the inlet speed of the cooling medium in each cooling medium ring 91 to enable the inner sides of the cooling medium rings 91 to form different temperature areas, so that a temperature gradient is formed in a heating cavity, and the temperature in the heating cavity gradually decreases from top to bottom; the upper end part of the heating cavity is a melting heating area, and the raw material 6 is placed in the melting heating area; the temperature in the melting heating zone is heated to 1238 ℃ and above to melt the raw material 6. Wherein, the area 1/2 of the upper part of the heating cavity is a melting heating area. The temperature gradient in the heating chamber is 5-15 k/cm.
Step three, the furnace body 7 is driven to ascend by the lifting driving device 1, and after the raw material 6 is subjected to a shouldering process, an isodiametric process and an annealing process, the growth of gallium arsenide single crystals is completed.
In this step, the shoulder stage occurs at the early stage of crystal growth, immediately after the seed crystal 5 comes into contact with the melt and begins to form crystals. At this stage, the diameter of the crystal increases rapidly, forming a wider portion resembling a shoulder. The purpose of the shoulder is to rapidly increase the cross-sectional area of the crystal to support subsequent longer isodiametric growth while also helping to reduce the propagation of defects, such as dislocations, in the crystal. By controlling the temperature gradient and growth rate, the shoulder rate and size of the crystal can be effectively managed. In this process, it is important to control the moving speed of the furnace body 7.
The isodiametric growth is the core stage of crystal growth, and is performed after the shouldering process. At this stage, by precisely controlling the growth conditions, the diameter of the crystal is kept relatively constant, thereby forming a uniform, straight columnar structure. The key to maintaining constant diameter growth is to balance the supersaturation of the melt and the shape of the crystal interface, ensuring uniform expansion of the crystal along a predetermined direction. This stage is particularly important for obtaining high quality single crystal materials. Also, in this process, the control of the moving speed of the furnace body 7 is also important.
Annealing is a heat treatment step after the completion of crystal growth in order to eliminate or reduce stress and defects inside the crystal. By slowly heating the crystal to a specific temperature and holding it for a period of time, and then slowly cooling, the atoms within the crystal can be encouraged to rearrange, eliminate irregularities in the microstructure, and improve the overall integrity, electrical and optical properties of the crystal. Annealing can reduce dislocation density and improve crystalline quality, which is a critical step in improving device performance for the semiconductor material gallium arsenide.
In the invention, the moving speed in the shoulder placing process is 1-2mm/h; the moving speed in the constant diameter process is 2-4mm/h. In the annealing process, the furnace body 7 does not move, and the cooling speed of the furnace body 7 in the annealing process is 50-150 ℃/h.
The invention has the following advantages:
1. in the invention, only the flow rate of the cooling medium in each cooling medium ring 91 is controlled, so that the temperature of different position areas in the heating cavity can be adjusted, and a required temperature gradient can be formed in the heating cavity, thereby ensuring the crystallization quality of the gallium arsenide single crystal and reducing the defects of the gallium arsenide single crystal.
2. When gallium arsenide monocrystal is prepared, the furnace body 7 moves but the raw material 6 does not move, so that the phenomenon that the crystal is disturbed in the process of growing gallium arsenide to influence the final crystallization quality can be effectively avoided.
The present application is not limited to the above-mentioned preferred embodiments, and any person who can obtain other various products under the teaching of the present application can make any changes in shape or structure, and all the technical solutions that are the same or similar to the present application fall within the scope of the present application.
Claims (10)
1. The gallium arsenide monocrystal growing device is characterized by comprising a furnace body and a raw material accommodating device for accommodating raw materials, wherein the furnace body is arranged on a lifting driving device, a heating cavity is arranged in the furnace body, the lower end of the heating cavity is open, a heating part is arranged on the inner wall of the furnace body, a plurality of cooling medium rings arranged along the vertical direction are arranged in the heating cavity, a cooling medium cavity is arranged in the cooling medium ring, and a cooling medium inlet pipe and a cooling medium outlet pipe which are communicated with the cooling medium cavity are connected to the cooling medium ring;
When the cooling medium is introduced into the cooling medium ring, the cooling medium exchanges heat with the area around the cooling medium ring to regulate the temperature of the area around the cooling medium ring.
2. The gallium arsenide single crystal growth apparatus according to claim 1, wherein the cooling medium ring is position-adjustable in a vertical direction; the cooling medium inlet pipe and the cooling medium outlet pipe pass through the upper end of the furnace body.
3. The gallium arsenide single crystal growing apparatus according to claim 1, wherein the lower end of the cooling medium inlet pipe is connected to the inner side of the cooling medium ring through a transition pipe, and the lower end of the cooling medium outlet pipe is connected to the inner side of the cooling medium ring through a transition pipe.
4. The gallium arsenide single crystal growing apparatus according to claim 2, wherein the upper end of the furnace body is provided with a through hole through which a cooling medium inlet pipe or a cooling medium outlet pipe can pass, the periphery of the through hole is provided with a mounting groove, and a clamping piece is arranged in the mounting groove; the clamping piece comprises a fixed ring and a plurality of thermal bending pieces, the fixed ring is fixedly arranged in the mounting groove, one end of each thermal bending piece is connected with the fixed ring, and the other end of each thermal bending piece is provided with a contact part; the thermal bending piece is arranged in a circular array and consists of a first metal layer and a second metal layer, the first metal layer is positioned on the outer side of the second metal layer, and the thermal expansion coefficient of the first metal layer is larger than that of the second metal layer; a cooling medium inlet pipe or a cooling medium outlet pipe passes through the space between the hot bent sheets on the clamping piece; when the temperature of the hot bent piece increases, the end of the hot bent piece provided with the contact part bends towards the center direction of the cooling medium inlet pipe or the cooling medium outlet pipe.
5. The gallium arsenide single crystal growth apparatus of claim 1, wherein the cooling medium is one of nitrogen, argon, and carbon dioxide.
6. The gallium arsenide single crystal growth apparatus according to claim 1, wherein the heating means is a heating wire, and the heating wire is arranged in a spiral shape.
7. The gallium arsenide single crystal growth apparatus according to claim 4, wherein the raw material containing means comprises a crucible, a vacuum vessel body, and a vacuum vessel cover, wherein the raw material is placed in the crucible, the crucible is placed in the vacuum vessel body, the vacuum vessel cover is hermetically connected to an upper end of the vacuum vessel body, and the interior of the vacuum vessel body is evacuated.
8. The gallium arsenide single crystal growth apparatus according to claim 7, wherein the crucible is a boron nitride crucible or a quartz crucible.
9. The gallium arsenide single crystal preparation method based on the gallium arsenide single crystal growth device of claim 7, comprising the following specific steps:
firstly, placing raw materials into a crucible, then placing the crucible into a vacuum container main body, mounting a vacuum container cover at the upper end of the vacuum container main body, and then vacuumizing the vacuum container main body;
Step two, placing a raw material accommodating device filled with raw materials below the furnace body, driving the furnace body to descend to a heating initial position through a lifting driving device, and completely positioning the raw material accommodating device in a heating cavity in the furnace body at the moment;
Starting a heating part, introducing cooling medium into the cooling medium rings through cooling medium inlet pipes, and regulating the inlet speed of the cooling medium in each cooling medium ring to enable the inner sides of the cooling medium rings to form different temperature areas, so that a temperature gradient is formed in a heating cavity, and the temperature in the heating cavity gradually decreases from top to bottom; the upper end part of the heating cavity is a melting heating area, and the raw materials are placed in the melting heating area; heating the temperature in the melting heating zone to 1238 ℃ and above to melt the feedstock;
Step three, driving the furnace body to ascend through the lifting driving device, and finishing the growth of gallium arsenide monocrystal after the raw materials undergo a shouldering process, an isodiametric process and an annealing process.
10. The method for producing a gallium arsenide single crystal according to claim 9, wherein the moving speed in the shouldering process is 1-2mm/h; the moving speed in the constant diameter process is 2-4mm/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410627086.4A CN118207628A (en) | 2024-05-21 | 2024-05-21 | Gallium arsenide monocrystal growing device and preparation method |
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