CN215050847U - In-furnace raw material injection device in crystal growth process - Google Patents

In-furnace raw material injection device in crystal growth process Download PDF

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Publication number
CN215050847U
CN215050847U CN202120712133.7U CN202120712133U CN215050847U CN 215050847 U CN215050847 U CN 215050847U CN 202120712133 U CN202120712133 U CN 202120712133U CN 215050847 U CN215050847 U CN 215050847U
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raw material
crystal growth
injection
furnace
water
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王书杰
孙聂枫
史艳磊
邵会民
徐森锋
付莉杰
王阳
李晓岚
欧欣
宋瑞良
刘惠生
孙同年
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CETC 13 Research Institute
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CETC 13 Research Institute
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Abstract

The utility model provides a raw materials injection apparatus in crystal growth in-process stove, belongs to the single crystal preparation field, concretely relates to crystal growth device, in particular to at the crystal growth in-process, sets up the raw materials injection apparatus in the furnace body. The device comprises an annular raw material water-cooling disc and a raw material bearing injection system; the raw material bearing and injecting system comprises a raw material bearing device, a resistance wire arranged around the raw material bearing device, a raw material injecting pipe communicated with the raw material bearing device and a raw material bearing device upper cover; the feedstock-bearing injection system is inserted into the feedstock vessel. Adopt the utility model discloses, can place the required partial raw and other materials of crystal growth in the raw materials bears, when the crystal growth material in the crucible is about to exhaust, the raw materials bears injection system and pours into the raw materials into the crucible, keeps the crystal to continue to grow. When large-size crystals grow, a crucible with small volume can be used, the temperature field in the crucible is easy to control, and the quality of the crystals is ensured.

Description

In-furnace raw material injection device in crystal growth process
Technical Field
The utility model belongs to the single crystal preparation field, concretely relates to crystal growth device, in particular to at the crystal growth in-process, set up the raw materials injection device in the furnace body.
Background
As a semiconductor material, the growth of a single crystal requires a high-temperature and high-pressure environment. Currently, the growth of the crystal is completed in a closed fixed space.
The large-size single crystal can prepare more large-size semiconductor single crystal substrates as much as possible, so that the cost of subsequent devices can be greatly reduced, and almost all semiconductor single crystals are developed towards the direction of large-size and long single crystals at present.
When the crystal grows to make a large-size crystal, the required raw materials are increased correspondingly. One means of increasing the raw material is to increase the crucible volume, with the problem that the temperature field inside the crucible is difficult to control.
To address this problem, there are two current solutions: a plurality of crucibles are used for feeding materials, and a feeding device is added outside the furnace body.
Chinese patent 200310108634.0 discloses an apparatus and method for melt replenishment of growing crystals using multiple communicating crucibles to increase the supply of feedstock in a manner that greatly increases the volume of the furnace body.
Chinese patent 201621248917.4 discloses a crystal growth furnace capable of realizing continuous production, in which a plurality of crucible assemblies are sequentially moved into the furnace body by a horizontal moving mechanism and a vertical lifting mechanism, which may interrupt the growth process of the crystal and affect the quality of the crystal.
Chinese patent 201720922581.3 discloses a material supply apparatus and a crystal growth system using another technical route, and discloses a material supply apparatus for supplying material from the outside to a crucible inside a furnace body. The two devices are connected, so that the complexity of device control is increased; the feeding from the outside of the furnace body may cause the pollution of the material in the feeding process.
Disclosure of Invention
To the above problem, the utility model provides a raw materials injection device in the crystal growth in-process stove.
In order to achieve the above object, the utility model adopts the following technical scheme: the utility model provides a raw materials injection device in crystal growth in-process stove, sets up crucible top in the crystal growth stove, and the key lies in:
the device comprises an annular raw material water-cooling disc and a raw material bearing injection system.
Evenly set up raw materials groove on the raw materials water-cooling dish, at raw materials water-cooling dish inboard, every raw materials groove is supporting to be set up the injection pipe groove.
The raw material bearing and injecting system comprises an insulating layer, a raw material bearing device, a resistance wire arranged around the raw material bearing device and a raw material injecting pipe communicated with the raw material bearing device.
The raw material loading injection system is inserted into the raw material tank, and the raw material injection pipe is extended out of the injection pipe tank.
Has the advantages that: adopt the utility model discloses, can place the required partial raw and other materials of crystal growth in the raw materials bears, when the crystal growth material in the crucible is about to exhaust, the raw materials bears injection system and pours into the raw materials into the crucible, keeps the crystal to continue to grow. When large-size crystals grow, a crucible with small volume can be used, the temperature field in the crucible is easy to control, and the quality of the crystals is ensured.
The cooling of the bearing injection system can be realized in the device, and the raw materials are prevented from melting and flowing out or being heated and sublimated; a plurality of bearing injection systems can be arranged in the device to realize continuous synthesis or intermittent synthesis; it is also possible to provide a load-bearing injection system for the two raw materials, which allows continuous synthesis or batch synthesis in the crucible. The crystal growth can be carried out in a smaller crucible through continuous synthesis, then the synthesis is stopped after the synthesis reaches the required melt amount, and then the crystal growth is carried out again through synthesis, so that the preparation of long single crystal is realized alternately, and meanwhile, energy and related consumables are saved.
Drawings
Figure 1 is a schematic diagram of the composition of the present invention,
figure 2 is a schematic diagram of the structure of a feedstock-bearing injection system,
figure 3 is a schematic view of the construction of a material carrier jacket,
figure 4 is a cross-sectional view of a feed water-cooled pan,
figure 5 is a top view of a feed water-cooled pan,
FIG. 6 is a raw material water-cooled tray cover.
Wherein, 1: a crystal growth furnace; 1-1: a partition plate; 6: a seed rod; 24: a crucible; 27: a raw material water-cooling disc; 27-1: a raw material tank; 27-2: injecting into a pipe groove; 27-3: a raw material water-cooling disc cover; 28: a feedstock-bearing injection system; 28-2: a feedstock carrier; 28-3: raw materials; 28-4: a resistance wire; 28-5: a raw material injection pipe; 32 waterway connection pads; 28-6: a raw material carrier upper cover; 28-7: an insulating layer upper cover; 28-8: a wire guide hole; 28-9: an insulating layer outer cylinder; 28-10: an injection pipe placing groove; 28-11: and an insulating layer baffle.
In the figure, the crystal growth furnace 1 is shown only partially.
Detailed Description
The present invention will be further explained with reference to the accompanying drawings.
A raw material injection device in a crystal growth process furnace is arranged above a crucible 24 in a crystal growth furnace 1. The apparatus comprises an annular feedstock water-cooled disc 27 and a feedstock-carrying injection system 28, as shown in figure 1.
A circulating water path is arranged in the crystal growth furnace 1; the raw material water cooling disc 27 is made of a copper material, is internally provided with a circulating water path, is provided with an outlet and an inlet of circulating water, is communicated with the circulating water path inside the crystal growth furnace 1, and is of a common water cooling structure.
The partition plate 1-1 is a part of the crystal growth furnace 1, and can withstand high temperature because of a circulating water path connected to the crystal growth furnace 1. The circulating water in the partition board 1-1 is sent to a circulating water path of the raw material water-cooling disc 27 through a water path connecting pad 32, and two pipelines are arranged in the middle of the water path connecting pad 32 and are used for connecting the circulating water inlet and outlet of the partition board 1-1 and the raw material water-cooling disc 27.
The above is a common design structure, which is not shown in the figures.
Referring to FIGS. 4 to 6, the raw material water-cooling plate 27 is ring-shaped, and has an outer diameter smaller than the inner diameter of the crystal growth furnace 1 and an inner diameter equal to or smaller than the inner diameter of the crucible 24, and 6 to 12 raw material tanks 27-1 are uniformly arranged thereon; an injection pipe groove 27-2 is arranged inside the raw material water-cooling disc 27 in a matched manner in each raw material groove 27-1; the raw material water-cooling disc 27 is also provided with a matched raw material water-cooling disc cover 27-3.
The raw material tank 27-1 may be cylindrical, and may be a through hole penetrating the raw material water-cooling tray 27 or a hole not penetrating the raw material water-cooling tray 27. In order to reduce the influence of the thermal field of the crucible below, the source material tank 27-1 is not a tube perforation in this embodiment.
The thickness of the water-cooled copper wall in the raw material water-cooled disc 27 is 10-15 mm.
The injection pipe tank 27-2 starts from the top of the raw material tank 27-1 and has a length greater than 4/5 of the height of the raw material water-cooled tray 27.
Referring to fig. 1 and 2, the raw material carrier injection system 28 comprises a raw material carrier 28-2, a resistance wire 28-4 arranged around the raw material carrier 28-2, a raw material injection pipe 28-5 communicated with the raw material carrier 28-2, and a raw material carrier upper cover 28-6.
Referring to fig. 3, the raw material bearing and injecting system 28 further comprises an outer sleeve of the raw material bearing device 28-2, the main body of the outer sleeve is an insulating layer outer cylinder 28-9, the top of the insulating layer outer cylinder 28-9 is open, and an insulating layer upper cover 28-7 with a wire guide hole 28-8 is arranged in a matched manner; the side surface of the insulating layer outer cylinder 28-9 is provided with an injection pipe placing groove 28-10 which is matched with an insulating layer baffle 28-11; the raw material carrier 28-2 is placed in the insulating layer outer cylinder 28-9, and the raw material injection tube 28-5 is protruded from the injection tube placing groove 28-10.
The raw material injection pipe 28-5 is disposed at the bottom of the raw material carrier 28-2 to facilitate the injection of the liquid raw material.
The raw material injection pipes 28-5 are set to 2 lengths, and the outlet of the raw material injection pipe is higher than and lower than the liquid level height of the reaction melt in the crystal growth process respectively, so that the injection requirements of liquid and gaseous raw materials are met.
The height of the raw material water-cooling disc 27 is 40-60mm higher than that of the raw material carrier 28-2, the inner part of the raw material groove 27-1 is a cylinder, the circle center distance between adjacent raw material grooves 27-1 is larger than D +40mm, and D is the diameter of the raw material groove 27-1.
The raw material carrying and injecting system 28 is inserted into the raw material tank 27-1, and the raw material water-cooling tray cover 27-3 covers the raw material water-cooling tray 27. The source material injection tube 28-5 protrudes from the injection tube slot 27-2 and is aligned with the underlying crucible 24. Because the inner diameter of the raw material water-cooling disc 27 is less than or equal to the inner diameter of the crucible 24, the raw material injection pipe 28-5 can be ensured to be aligned with the crucible 24, and the raw material does not leak.
And (5) working process of the equipment.
The number of feedstock-bearing injection systems 28 is determined based on the number of feedstock channels 27-1 and the amount of feedstock required.
The crystal growth feedstock 28-3 is placed in the feedstock carrier 28-2 and the feedstock carrier top lid 28-6 is welded to the feedstock carrier 28-2. The material carrier upper cover 28-6 and the material carrier 28-2 are made of quartz.
The resistance wire 28-4 is wound outside the raw material carrier 28-2 and put into the insulating layer outer cylinder 28-9 together, the raw material injection pipe 28-5 is assembled in the injection pipe placing groove 28-10, and the insulating layer baffle 28-11 is inserted into the injection pipe placing groove 28-10 and assembled together.
The two-pole leads of the resistance wire 28-4 are passed through two lead holes 28-8 (not shown) in the insulating layer cover 28-7.
When two materials are required, such as phosphorus and indium for growing an indium phosphide crystal, one half of the feedstock carrying injection system 28 is charged with phosphorus and the other half is charged with indium.
If the raw material 28-3 is supplied in a gaseous state (e.g., phosphorus), the port of the raw material injection tube 28-5 is to be introduced into the reaction melt; if liquid (e.g., indium), the end of the source material injection tube 28-5 is above the reaction melt level.
Placing the feedstock carrying injection system 28 in the feedstock tank 27-1; if the two raw materials are used, the raw materials are arranged at intervals according to the types of the raw materials.
The raw material water-cooling disc 27 is connected to the partition plate 1-1 through a waterway connection pad 32.
The crucible 24 is filled with a crystal growth material, a seed crystal is fitted to the seed rod 6, and the crucible is heated to start crystal growth.
When raw materials need to be added, the resistance wire 28-4 is controlled to heat one or two bearing injection systems 28, liquid or gas phase materials are changed and injected into the crucible to form new reaction melt, and the growth of crystals is continued.
When the feedstock in one or a group of carrier injection systems 28 is exhausted, the next or a next group is activated, and the process is alternated to produce a long single crystal until all of the feedstock 28-3 in the carrier injection system 28 is exhausted.

Claims (10)

1. The utility model provides a raw materials injection device in crystal growth in-process stove, sets up crucible (24) top in crystal growth stove (1), its characterized in that:
the apparatus comprises an annular raw material water-cooled disc (27) and a raw material bearing injection system (28);
raw material grooves (27-1) are uniformly arranged on the raw material water-cooling disc (27), and injection pipe grooves (27-2) are arranged on the inner side of the raw material water-cooling disc (27) in a matched manner in each raw material groove (27-1);
the raw material bearing and injecting system (28) comprises a raw material bearing device (28-2), a resistance wire (28-4) arranged around the raw material bearing device (28-2), a raw material injecting pipe (28-5) communicated with the raw material bearing device (28-2) and a raw material bearing device upper cover (28-6);
the raw material carrying injection system (28) is inserted into the raw material tank (27-1), and the raw material injection pipe (28-5) protrudes from the injection pipe tank (27-2).
2. The in-furnace raw material injection apparatus in a crystal growth process according to claim 1, characterized in that: the outer diameter of the raw material water-cooling disc (27) is smaller than the inner diameter of the crystal growth furnace (1), and the inner diameter of the raw material water-cooling disc (27) is smaller than or equal to the inner diameter of the crucible (24).
3. The apparatus for injecting a raw material into a furnace for crystal growth according to claim 1 or 2, wherein the raw material water-cooling plate (27) is made of copper and has a wall thickness of 10 to 15 mm.
4. The in-furnace raw material injection apparatus for crystal growth according to claim 1 or 2, characterized in that: the raw material tanks (27-1) are provided with 6-12.
5. The in-furnace raw material injection apparatus for crystal growth according to claim 1 or 2, characterized in that: the length of the injection tube groove (27-2) is larger than 4/5 of the height of the raw material water-cooling disc (27).
6. The in-furnace raw material injection apparatus for crystal growth according to claim 1 or 2, characterized in that: the raw material water-cooling disc (27) also comprises a raw material water-cooling disc cover (27-3).
7. The in-furnace raw material injection apparatus in a crystal growth process according to claim 1, characterized in that: the raw material injection pipe (28-5) is arranged at the bottom of the raw material carrier (28-2).
8. The in-furnace raw material injection apparatus in a crystal growth process according to claim 1, characterized in that: the raw material injection pipes (28-5) are set to 2 lengths, respectively, the outlet of which is higher and lower than the liquid level of the reaction melt during the crystal growth.
9. The in-furnace raw material injection apparatus for crystal growth according to claim 7 or 8, wherein: the raw material bearing and injecting system (28) further comprises an outer sleeve of the raw material bearing device (28-2), the outer sleeve comprises an insulating layer outer cylinder (28-9), the top of the insulating layer outer cylinder (28-9) is open, and an insulating layer upper cover (28-7) with a wire guide hole (28-8) is arranged in a matched mode; the insulating layer outer cylinder (28-9) is provided with an injection pipe placing groove (28-10) which is matched with an insulating layer baffle (28-11); the raw material carrier (28-2) is placed in the insulating layer outer cylinder (28-9).
10. The in-furnace raw material injection apparatus in a crystal growth process according to claim 1, characterized in that: the height of the raw material water-cooling disc (27) is 40-60mm higher than that of the raw material carrier (28-2), the interior of the raw material groove (27-1) is a cylinder, the distance between the circle centers of adjacent raw material grooves (27-1) is greater than D +40mm, and D is the diameter of the raw material groove (27-1).
CN202120712133.7U 2021-04-08 2021-04-08 In-furnace raw material injection device in crystal growth process Active CN215050847U (en)

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CN202120712133.7U CN215050847U (en) 2021-04-08 2021-04-08 In-furnace raw material injection device in crystal growth process

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022213643A1 (en) * 2021-04-08 2022-10-13 中国电子科技集团公司第十三研究所 Large-scale compound semiconductor single crystal growth system and method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022213643A1 (en) * 2021-04-08 2022-10-13 中国电子科技集团公司第十三研究所 Large-scale compound semiconductor single crystal growth system and method

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