CN210620996U - Furnace body temperature adjustable cold wall single crystal furnace - Google Patents

Furnace body temperature adjustable cold wall single crystal furnace Download PDF

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CN210620996U
CN210620996U CN201921569220.0U CN201921569220U CN210620996U CN 210620996 U CN210620996 U CN 210620996U CN 201921569220 U CN201921569220 U CN 201921569220U CN 210620996 U CN210620996 U CN 210620996U
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furnace
wall
temperature
cold
single crystal
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柴晓磊
高佑君
樊海强
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Shanxi Zhongke Crystal Electric Information Material Co Ltd
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Shanxi Zhongke Crystal Electric Information Material Co Ltd
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Abstract

The utility model relates to the technical field of semiconductor material preparation, in particular to a cold wall single crystal furnace with an adjustable furnace body temperature, which comprises a crystal growing device and a constant temperature cold fireplace, wherein the crystal growing device is arranged in the constant temperature cold fireplace; the specific temperature field of crystal growth is realized by controlling the temperature of the constant-temperature cold wall furnace and the pressure in the furnace; the crystal single crystal rate is improved to 75% from 60% after the constant temperature cold fireplace is adopted to avoid the influence of the environment on the crystal growth temperature field; the phenomena of pipe expansion, pipe contraction and the like of a quartz pipe are avoided by adopting the constant-temperature cold fireplace through controlling the pressure in the furnace, the actual arsenic pressure is consistent with the set arsenic pressure, and crystals are longitudinally and uniformly promoted; by regulating and controlling the temperature reduction program, the annealing period is shortened from the original 140h to 116 h. The crystal growth period is shortened, and the economic benefit is improved.

Description

Furnace body temperature adjustable cold wall single crystal furnace
Technical Field
The utility model relates to a semiconductor material preparation technical field, more specifically relate to a furnace body temperature adjustable cold wall single crystal growing furnace.
Background
Gallium arsenide (GaAs), which is a iii-v group compound semiconductor, is formed by combining two elements of arsenic and gallium, has a bright gray appearance, a metallic luster, and a brittle and hard appearance, is the most mature second-generation compound semiconductor material internationally recognized in the present generation, has superior characteristics of high frequency, high electron mobility, high output power, low noise, good linearity and the like, is the most important compound semiconductor material, which is next to silicon, because gallium arsenide (GaAs) is the most important compound semiconductor material because of the largest production and the most wide application at present. Due to the excellent performance and energy band structure, the gallium arsenide material has great development potential in the aspects of microwave devices, light-emitting devices and the like. The advanced production technology of the gallium arsenide material is still mastered in international companies such as Japan, Germany and the United states, and compared with foreign companies, domestic enterprises have a larger gap in the production technology of the gallium arsenide material.
The gallium arsenide single crystal industrialized growth process mainly comprises the following steps: the liquid seal Czochralski method (LEC), the horizontal British Raman method (HB), the vertical British Raman method (VB), the vertical gradient solidification method (VGF) and the like, wherein the vertical gradient solidification method has the advantages of low equipment manufacturing cost and easy realization of program control, the grown single crystal has a plurality of advantages of lower dislocation density, higher integrity, uniformity and the like, and the growth environment of the VGF growth furnace is in a room temperature environment. Along with the improvement of the requirement on the crystal quality, the change of the environmental temperature and the humidity causes temperature fluctuation to the temperature field, thereby causing the fluctuation of the quality of the gallium arsenide crystal. The pressure in the quartz tube can only be about 1 atmosphere, otherwise the quartz tube can be damaged.
SUMMERY OF THE UTILITY MODEL
In order to overcome the defects in the prior art, the utility model provides a cold wall single crystal furnace with adjustable furnace body temperature, which provides a crystal growth environment without being influenced by environmental change for the crystal growth by controlling the atmosphere and the pressure in the cold wall of a constant temperature cold fireplace and the furnace.
In order to solve the technical problem, the utility model discloses the technical scheme who adopts is:
a cold wall single crystal furnace with an adjustable furnace body temperature comprises a crystal growing device and a constant temperature cold wall furnace, wherein the crystal growing device is arranged in the constant temperature cold wall furnace; the crystal growth device comprises a PBN crucible, a quartz tube and a heater, wherein the PBN crucible is fixed in the quartz tube, a quartz cap is arranged in the quartz tube, the quartz tube is placed on a furnace core, and a glass rod is arranged in the furnace core; a heat preservation device is arranged outside the crystal growth device, the heat preservation device is of a hollow cylindrical structure with an opening at the lower part, a heater is embedded in the inner wall of the heat preservation device, and gaps are formed among the heater, the quartz tube and the furnace core; the constant-temperature cold fireplace comprises a top wall, a side wall and a bottom wall, wherein the top wall, the side wall and the bottom wall are of hollow structures, cooling media are arranged inside the top wall, the side wall and the bottom wall respectively, and the temperature and the flow of the cooling media can be controlled through the outside. The temperature of the system is controlled by controlling the temperature of the cooling medium, and the flow control of the cooling medium in the cold fireplace is realized by controlling the water inlet pressure of the cooling medium.
Further, the heaters are arranged in six groups.
Further, the heater temperatures are independently operated, respectively.
Further, the constant-temperature cold fireplace is further provided with an air pressure control system, and the air pressure control system comprises an air inlet valve, an air outlet valve and an air pressure control device.
Furthermore, the temperature and the flow of the cooling medium in the top wall, the side wall and the bottom wall are respectively and independently controlled.
Furthermore, the side walls are arranged into 1-3 groups, a plurality of groups of side walls are overlapped up and down, and adjacent side walls are fixedly connected. The multiple side walls can effectively control the heat dissipation path.
Furthermore, the temperature and the flow of the cooling medium in the side wall are respectively and independently controlled.
Compared with the prior art, the utility model discloses the beneficial effect who has does:
the utility model provides a cold wall single crystal furnace with an adjustable furnace body temperature, which realizes the thermal radiation heating of a furnace core, a crucible furnace and a quartz tube through six groups of heaters, and the six groups of heaters independently operate to realize the heating of different temperatures at different parts; providing a heat loss channel through the bottom glass rod; the specific temperature field of crystal growth is realized by controlling the temperature of the constant-temperature cold wall furnace and the pressure in the furnace, so that the influence of environmental change on the heat dissipation of the crystal furnace is avoided, and the consistency of the internal and external pressures of the quartz tube is ensured; the crystal single crystal rate is improved to 75% from 60% after the constant temperature cold fireplace is adopted to avoid the influence of the environment on the crystal growth temperature field; the phenomena of pipe expansion, pipe contraction and the like of the quartz tube are avoided by adopting the constant-temperature cold fireplace through controlling the pressure in the furnace, and the actual arsenic pressure is consistent with the set arsenic pressure; by regulating and controlling the temperature reduction program, the annealing period is shortened from the original 140h to 116 h. The crystal growth period is shortened, and the economic benefit is improved.
Drawings
FIG. 1 shows a cold wall single crystal furnace with an adjustable furnace body temperature provided by the utility model.
FIG. 2 is a schematic view of a crystal growth apparatus
In the figure: 1 is PBN crucible, 2 is quartz tube, 3 is heater, 4 is quartz cap, 5 is furnace core, 6 is glass rod, 7 is heat preservation device, 8 is roof, 9 is lateral wall, 10 is bottom wall, 11 is admission valve, 12 is air outlet valve.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
As shown in fig. 1-2, comprises a crystal growing device and a constant temperature cold fireplace, wherein the crystal growing device is arranged in the constant temperature cold fireplace; the crystal growth device comprises a PBN crucible 1, a quartz tube 2 and a heater 3, wherein the PBN crucible 1 is fixed in the quartz tube 2, a quartz cap 4 is arranged in the quartz tube 2, the quartz tube 2 is placed on a furnace core 5, and a glass rod 6 is arranged in the furnace core; a heat preservation device 7 is arranged outside the crystal growth device, the heat preservation device 7 is a hollow cylindrical structure with an opening at the lower part, and a heater 3 is embedded in the inner wall of the heat preservation device 7; the constant-temperature cold fireplace comprises a top wall 8, a side wall 9 and a bottom wall 10, wherein the top wall 8, the side wall 9 and the bottom wall 10 are sealed through rubber strips when being closed; the top wall 8, the side wall 9 and the bottom wall 10 are of hollow structures, cooling media are arranged inside the top wall, the side wall and the bottom wall respectively, and the temperature and the flow of the cooling media can be controlled through the outside. The heaters 3 are arranged into six groups, and the six groups of heaters operate independently to realize different temperature control of different parts. The constant-temperature cold fireplace is further provided with an air pressure control system, the air pressure control system comprises an air inlet valve 11, an air outlet valve 12 and an air pressure control device, and the air pressure control system controls the air pressure in the constant-temperature cold fireplace by controlling the air inlet of the air inlet valve 11 and the air outlet valve 12 to be discharged. The temperature and the flow of the cooling medium in the top wall 8, the side wall 9 and the bottom wall 10 are respectively and independently controlled. The side walls 9 are arranged into 1-3 groups, a plurality of groups of side walls 9 are vertically stacked, and the adjacent side walls 9 are fixedly connected. The plurality of side walls 9 effectively control the heat dissipation path. The temperature and the flow of the cooling medium in the side wall 9 are respectively and independently controlled. And a bearing support device is arranged in the constant-temperature cold wall furnace through the bottom and is used for placing a crystal growth device.
In this embodiment, the method for growing gallium arsenide crystals by using a cold-wall single crystal furnace with an adjustable furnace body temperature comprises the following steps:
s1, fixing the seed crystal on the cone of the PBN crucible 1, and putting the GaAs polycrystalline material into the PBN crucible 1;
s2, placing the PBN crucible 1 into a quartz tube 2, covering a quartz cap 4 on the upper end of the PBN crucible 1, vacuumizing, and sealing and welding the quartz cap 4 and the PBN crucible 1 by oxyhydrogen flame;
s3, controlling the temperature of the furnace core 5 to be 1220 ℃, the temperature of the heater 3 to be 1250 ℃, and providing a stable temperature field by controlling the temperature of the constant-temperature cold fireplace in the crystal growth process; according to the pressure required by the quartz tube, the pressure in the quartz tube is the same as the pressure in the furnace by controlling the pressure adjustment of the constant-temperature cold fireplace;
s4, after the melting and inoculation of the top of the seed crystal are completed, controlling the growth rate of the crystal to be 0.5-5mm/h until all the crystal is crystallized.
Further, the temperature and pressure control of the constant-temperature wall cooling furnace is specifically as follows:
(1) controlling the temperature of the constant-temperature wall cooling furnace:
in the crystal growth blank period, the water inlet temperature of the constant-temperature cold fireplace is kept at 25 +/-0.1 ℃, the water inlet pressure is kept at 0.1MPa, and a stable crystal growth environment which does not change along with the environment is stably and constantly provided;
in the equal-diameter growth and ending period of the crystal, the fluid water inlet pressure at the lower parts of the bottom wall 10 and the side wall 9 of the constant-temperature cold fireplace is gradually increased to 0.5MPa, the fluid water inlet pressure of other pipelines is maintained at 0.1MPa, the water temperature of inlet water is unchanged, only the heat quantity of the bottom is increased, and a stable growth interface required by the crystal growth is maintained;
in the crystal cooling period, the fluid inlet pressure in the top wall 7 of the constant-temperature cold fireplace is increased to 0.5MPa, and the pressure of other cooling water paths is kept unchanged;
(2) pressure control of the constant-temperature cold fireplace:
a temperature rise period: the pressure in the cold fireplace is increased along with the rise of the arsenic pressure in the quartz tube, the pressure of the cold fireplace is set to be the saturated vapor pressure of the arsenic at the temperature, and when the arsenic amount required for maintaining the pressure at the temperature in the quartz tube exceeds the arsenic addition amount, the pressure in the furnace is set according to the arsenic addition amount so as to maintain the balance of the internal and external pressures of the quartz tube;
crystal growth period: the pressure in the furnace is maintained at a constant pressure according to the requirement of the pressure in the quartz tube;
and (3) crystal cooling period: the pressure in the furnace is reduced along with the reduction of the pressure of the arsenic vapor in the quartz tube, and the balance of the pressure inside and outside the quartz tube is maintained.
The above description has been made in detail only for the preferred embodiment of the present invention, but the present invention is not limited to the above embodiment, and various changes can be made without departing from the spirit of the present invention within the knowledge scope of those skilled in the art, and all such changes are intended to be encompassed by the present invention.

Claims (7)

1. A furnace body temperature adjustable cold wall single crystal growing furnace which is characterized in that: the device comprises a crystal growth device and a constant-temperature cold fireplace, wherein the crystal growth device is arranged in the constant-temperature cold fireplace; the crystal growth device comprises a PBN crucible (1), a quartz tube (2) and a heater (3), wherein the PBN crucible (1) is fixed in the quartz tube (2), a quartz cap (4) is arranged in the quartz tube (2), the quartz tube (2) is placed on a furnace core (5), and a glass rod (6) is arranged in the furnace core; a heat preservation device (7) is arranged outside the crystal growth device, the heat preservation device (7) is of a hollow cylindrical structure with an opening at the lower part, and a heater (3) is embedded in the inner wall of the heat preservation device (7); the constant-temperature cold fireplace comprises a top wall (8), a side wall (9) and a bottom wall (10), wherein the top wall (8), the side wall (9) and the bottom wall (10) are sealed through rubber strips when closed; the top wall (8), the side wall (9) and the bottom wall (10) are of hollow structures, cooling media are arranged inside the top wall, the side wall and the bottom wall respectively, and the temperature and the flow of the cooling media can be controlled through the outside.
2. The cold wall single crystal furnace with the adjustable furnace body temperature according to claim 1, characterized in that: the heaters (3) are arranged into six groups.
3. The cold wall single crystal furnace with the adjustable furnace body temperature according to claim 1 or 2, characterized in that: the temperatures of the heaters (3) are respectively and independently operated.
4. The cold wall single crystal furnace with the adjustable furnace body temperature according to claim 1, characterized in that: the constant-temperature cold fireplace is further provided with an air pressure control system, and the air pressure control system comprises an air inlet valve (11), an air outlet valve (12) and an air pressure control device.
5. The cold wall single crystal furnace with the adjustable furnace body temperature according to claim 1, characterized in that: the temperature and the flow of the cooling medium in the top wall (8), the side wall (9) and the bottom wall (10) are respectively and independently controlled.
6. The cold wall single crystal furnace with the adjustable furnace body temperature according to claim 1, characterized in that: the side walls (9) are arranged into 1-3 groups, a plurality of groups of side walls (9) are vertically stacked, and the adjacent side walls (9) are fixedly connected.
7. The cold wall single crystal furnace with the adjustable furnace body temperature according to claim 1, characterized in that: the temperature and the flow of the cooling medium in the side wall (9) are respectively and independently controlled.
CN201921569220.0U 2019-09-20 2019-09-20 Furnace body temperature adjustable cold wall single crystal furnace Active CN210620996U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110565168A (en) * 2019-09-20 2019-12-13 山西中科晶电信息材料有限公司 Furnace body temperature-adjustable cold wall single crystal furnace and gallium arsenide crystal growth method
CN113061984A (en) * 2021-03-09 2021-07-02 山东天岳先进科技股份有限公司 Crystal growth method and device

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110565168A (en) * 2019-09-20 2019-12-13 山西中科晶电信息材料有限公司 Furnace body temperature-adjustable cold wall single crystal furnace and gallium arsenide crystal growth method
CN113061984A (en) * 2021-03-09 2021-07-02 山东天岳先进科技股份有限公司 Crystal growth method and device
CN113061984B (en) * 2021-03-09 2022-03-01 山东天岳先进科技股份有限公司 Crystal growth method and device

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