阅读说明：本技术 一种大尺寸晶体生长控制装置及控制方法 (Large-size crystal growth control device and control method ) 是由 马孙明 彭方 郭玉勇 窦仁勤 毛炯 陈仪翔 张庆礼 于 2020-07-17 设计创作，主要内容包括：本发明公开了一种大尺寸晶体生长控制装置及控制方法,属于晶体材料技术领域。一种大尺寸晶体生长控制装置,包括支架、控制器、电动伸缩杆、坩埚、加热套、供给箱和增压泵,控制器固定连接在支架的底部,加热套固定连接在支架的顶部,坩埚可拆卸套接在加热套内,支架上固定连接有支撑杆,电动伸缩杆固定连接在支撑杆上,电动伸缩杆的输出端固定连接有加热器,加热器的输出端固定连接有导热环,导热环延伸至坩埚内,电动增压泵固定连接在供给箱的侧壁,增压泵的输入端通过第一导管与供给箱相连通,增压泵的输出端通过第二导管与坩埚相连通；本发明利用加热套的通槽和壁厚顺序保证晶体的成型时,降低结晶块的多余应力,导热环降低脱离时的热冲击。(The invention discloses a large-size crystal growth control device and a control method, and belongs to the technical field of crystal materials. A large-size crystal growth control device comprises a support, a controller, an electric telescopic rod, a crucible, a heating sleeve, a supply box and a booster pump, wherein the controller is fixedly connected to the bottom of the support; the invention utilizes the through groove and the wall thickness sequence of the heating sleeve to ensure that the redundant stress of a crystal block is reduced and the thermal shock when the crystal is separated is reduced by the heat conducting ring.)

1. A large-size crystal growth control device comprises a support (1), a controller (101), an electric telescopic rod (2), a crucible (3), a heating sleeve (4), a supply box (5) and a booster pump (6), and is characterized in that the controller (101) is fixedly connected to the bottom of the support (1), the heating sleeve (4) is fixedly connected to the top of the support (1), the crucible (3) is detachably sleeved in the heating sleeve (4), a support rod (102) is fixedly connected to the support (1), the electric telescopic rod (2) is fixedly connected to the support rod (102), a heater (201) is fixedly connected to the output end of the electric telescopic rod (2), a heat conduction ring (202) is fixedly connected to the output end of the heater (201), the heat conduction ring (202) extends into the crucible (3), and the electric booster pump (6) is fixedly connected to the side wall of the supply box (5), the input end of the booster pump (6) is communicated with the supply box (5) through a first conduit (601), and the output end of the booster pump (6) is communicated with the crucible (3) through a second conduit (602).

2. The growth control device for the large-size crystals is characterized in that electrode support legs (401) are fixedly connected to the bottom of the heating jacket (4), and a through groove (402) is formed in the outer wall of the heating jacket (4).

3. A large size crystal growth control device according to claim 2, wherein said through slot (402) is shaped in particular as "W".

4. A large size crystal growth control apparatus as claimed in claim 1, wherein a flow meter is provided in said booster pump (6).

5. A large size crystal growth control device according to claim 1, characterized in that the top of the feed box (5) is provided with a feed pipe (501).

6. A large size crystal growth control device according to claim 1, characterized in that the top of the crucible (3) is provided with an air inlet pipe (301).

7. A control method applied to a large-size crystal growth control device as claimed in any one of claims 1 to 6, comprising the steps of:

step 1: cleaning the inner wall of the crucible (3) and drying;

step 2: starting a booster pump (6), extracting a proper amount of crystal materials from a supply box (5) through a first conduit (601), injecting the crystal materials into a closable crucible (3), and counting the supply amount through a flow meter arranged in the booster pump (6);

and step 3: placing cooled seed crystals in the crucible (3) and generating by adopting a kyropoulos method;

and 4, step 4: after the raw material injected into the crucible (3) reaches a set value, stopping the booster pump (6), and introducing inert gas into the closable crucible (3) through the gas inlet pipe (301);

and 5: electrifying the negative and positive electrode support legs (401) at the bottom of the heating sleeve (4) through the controller (101), thereby heating the heating sleeve (4) and controlling the melting time of the crystal material;

step 6: in the process of heating the heating sleeve (4), the top of the heating sleeve (4) is influenced by the W-shaped through groove (402), so that the temperature of the part deflected upwards is slightly lower than that of the bottom in the heating process, and the temperature of the crystal material in the crucible (3) is increased from the bottom to the top;

and 7: when the surface of the seed crystal and the raw material are molten, stopping heating, gradually cooling the crucible (3), and in the process of cooling the raw material, losing temperature at the bottom firstly, so as to ensure that the seed crystal is gradually crystallized from the bottom to the top to form crystals of a required sequence;

and 8: after crystallization is finished, discharging redundant gas, opening a sealing cover of the crucible (3), starting the electric telescopic rod (2) and the heater (201), heating the heat conduction ring (202), enabling the heat conduction ring (202) to surround the periphery of the crystallized block, enabling the crystallized block to be separated from the residual solution, and preventing larger thermal shock;

and step 9: extracting the crystal block and cleaning the inner wall of the crucible (3).

8. The method as claimed in claim 7, wherein the inert gas in step 4 is helium.

9. The method as claimed in claim 7, wherein the melting time in step 5 is maintained at 45-52 hours.

10. The method as claimed in claim 7, wherein the temperature reduction time in step 7 is maintained for 90 hours, and the temperature is in the range of 1800 ℃ to 2200 ℃.

Technical Field

The invention relates to the technical field of crystal materials, in particular to a large-size crystal growth control device and a control method.

Background

Sapphire is an alpha-phase single crystal of aluminum oxide, has high hardness (Mohs 9), is resistant to high temperature and corrosion, and has excellent light transmittance. The sapphire crystal is widely applied to the fields of semiconductor substrates, special windows and the like. Especially, the high-brightness white light LED is used as a next-generation general lighting device and has the advantages of green, energy saving and the like. The sapphire substrate is the most main substrate of the gallium nitride-based white light LED, the market demand is huge, the sapphire crystal is generally manufactured by adopting a mode of growing in molten liquid, and the most main growing modes comprise a kyropoulos method, a pulling method and a crucible descending method.

Disclosure of Invention

The invention aims to solve the defect that a crystal block is easy to generate thermal shock and damage in the prior art, and provides a large-size crystal growth control device and a control method.

In order to achieve the purpose, the invention adopts the following technical scheme:

the utility model provides a jumbo size crystal growth controlling means and control method, includes support, controller, electric telescopic handle, crucible, heating jacket, feed box and booster pump, controller fixed connection is in the bottom of support, heating jacket fixed connection is at the top of support, the crucible can be dismantled to cup joint in the heating jacket, fixedly connected with bracing piece on the support, electric telescopic handle fixed connection is on the bracing piece, electric telescopic handle's output fixedly connected with heater, the output fixedly connected with heat conduction ring of heater, heat conduction ring extends to in the crucible, electric booster pump fixed connection is at the lateral wall of feed box, the input of booster pump communicates with the feed box through first pipe, the output of booster pump is linked together with the crucible through the second pipe.

Preferably, the bottom of the heating sleeve is fixedly connected with electrode support legs, and the outer wall of the heating sleeve is provided with a through groove.

Preferably, the through-groove has a shape of "W".

Preferably, a flow meter is arranged in the booster pump.

Preferably, the feeding pipe is arranged at the top of the feeding box.

Preferably, the top of the crucible is provided with an air inlet pipe.

A control method comprising the steps of:

step 1: cleaning the inner wall of the crucible and drying;

step 2: starting a booster pump, extracting a proper amount of crystal materials from a supply box through a first conduit, injecting the crystal materials into a closable crucible, and counting the supply amount through a flow meter arranged in the booster pump;

and step 3: placing cooled seed crystals in a crucible, and generating by adopting a kyropoulos method;

and 4, step 4: stopping the booster pump after the raw material injected into the crucible reaches a set value, and introducing inert gas into the closable crucible through the gas inlet pipe;

and 5: electrifying the negative and positive electrode support legs at the bottom of the heating sleeve through a controller, thereby heating the heating sleeve and controlling the melting time of the crystal material;

step 6: in the heating process of the heating sleeve, the top of the heating sleeve is influenced by the W-shaped through groove, so that the temperature of the part deflected upwards is slightly lower than that of the bottom in the heating process, and the temperature of the crystal material in the crucible is increased from the bottom to the top;

and 7: stopping heating when the surface of the seed crystal and the raw material are molten, gradually cooling the crucible, and losing temperature at the bottom in the cooling process of the raw material, so that the seed crystal is ensured to be gradually crystallized from the bottom to the top to form a crystal of a required sequence;

and 8: after crystallization is finished, discharging redundant gas, opening a sealing cover of the crucible, starting an electric telescopic rod and a heater, heating a heat conduction ring, enabling the heat conduction ring to surround the periphery of the crystallized block, enabling the crystallized block to be separated from the residual solution, and preventing larger thermal shock;

and step 9: and extracting the crystal blocks and cleaning the inner wall of the crucible.

Preferably, the inert gas in step 4 is helium.

Preferably, the melting time in step 5 is maintained at 45-52 hours.

Preferably, the cooling time in the step 7 is maintained for 90 hours, and the temperature is in the range of 1800-2200 ℃.

Compared with the prior art, the invention provides a large-size crystal growth control device and a control method, which have the following beneficial effects:

1. according to the large-size crystal growth control device, the contact area between the heating sleeve and the crucible is controlled through the W-shaped through groove formed in the heating sleeve, so that the heating sequence of the crucible is effectively adjusted, the heating sleeve with the thick upper part and the thin lower part controls the cooling gradient of the crucible, the seed crystals can be crystallized sequentially in the crystallization process, the formation of the crystals is guaranteed, and the redundant partial stress of the subsequently extracted crystal blocks is reduced.

2. According to the large-size crystal growth control device and the control method, the temperature of the crystal around the crystal block is raised through the heat conduction ring, so that the stress connection between the crystal block and an unformed melt is reduced, excessive thermal shock generated when the crystal block is separated is prevented, and the sequence integrity of the interior of the extracted crystal block is ensured.

Drawings

FIG. 1 is a schematic structural diagram of a large-sized crystal growth control device according to the present invention;

FIG. 2 is a schematic structural diagram of a large-sized crystal growth control device crucible according to the present invention.

In the figure: 1. a support; 101. a controller; 102. a support bar; 2. an electric telescopic rod; 201. a heater; 202. a heat conducting ring; 3. a crucible; 301. an air inlet pipe; 4. heating a jacket; 401. an electrode support leg; 402. a through groove; 5. a supply tank; 501. a feed pipe; 6. a booster pump; 601. a first conduit; 602. a second conduit.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.

In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.

Referring to fig. 1-2, a large-size crystal growth control device and control method, comprising a support 1, a controller 101, an electric telescopic rod 2, crucible 3, heating jacket 4, supply box 5 and booster pump 6, controller 101 fixed connection is in the bottom of support 1, 4 fixed connection of heating jacket are at the top of support 1, crucible 3 can be dismantled and cup joint in heating jacket 4, fixedly connected with bracing piece 102 on the support 1, 2 fixed connection of electric telescopic handle are on bracing piece 102, 2 output fixedly connected with heaters 201 of electric telescopic handle, heater 201's output fixedly connected with heat-conducting ring 202, heat-conducting ring 202 extends to in crucible 3, 6 fixed connection of electric booster pump is at the lateral wall of supply box 5, the input of booster pump 6 is linked together through first pipe 601 and supply box 5, the output of booster pump 6 is linked together through second pipe 602 and crucible 3.

The bottom fixedly connected with electrode stabilizer blade 401 of heating jacket 4, logical groove 402 has been seted up to 4 outer walls of heating jacket, and the shape that leads to groove 402 specifically is "W", is provided with the flowmeter in the booster pump 6, and 5 tops of feed box are provided with inlet pipe 501, and the top of crucible 3 is provided with intake pipe 301.

A control method comprising the steps of:

step 1: cleaning the inner wall of the crucible 3 and drying;

step 2: starting a booster pump 6, extracting a proper amount of crystal materials from a supply box 5 through a first conduit 601, injecting the crystal materials into a closable crucible 3, and counting the supply amount through a flow meter arranged in the booster pump 6;

and step 3: placing cooled seed crystals in the crucible 3, and generating by adopting a kyropoulos method;

and 4, step 4: after the raw material injected into the crucible 3 reaches a set value, stopping the booster pump 6, and introducing inert gas into the closable crucible 3 through the gas inlet pipe 301;

and 5: electrifying the cathode and anode support legs 401 at the bottom of the heating jacket 4 through the controller 101, thereby heating the heating jacket 4 and controlling the melting time of the crystal material;

step 6: in the process of heating the heating jacket 4, the top of the heating jacket 4 is influenced by the W-shaped through groove 402, so that in the heating process, the temperature of the part deflected upwards is slightly lower than that of the bottom, and the temperature of the crystal material in the crucible 3 is increased from the bottom to the top;

and 7: stopping heating when the surface of the seed crystal and the raw material are molten, gradually cooling the crucible 3, and losing temperature at the bottom in the cooling process of the raw material, so that the seed crystal is ensured to be gradually crystallized from the bottom to the top to form a crystal of a required sequence;

and 8: after crystallization is finished, discharging redundant gas, opening a sealing cover of the crucible 3, starting the electric telescopic rod 2 and the heater 201, heating the heat conduction ring 202, enabling the heat conduction ring 202 to surround the periphery of the crystallized block, enabling the crystallized block to be separated from the residual solution, and preventing larger thermal shock;

and step 9: the ingot is extracted and the inner wall of the crucible 3 is cleaned.

The inert gas in the step 4 is helium.

The melting time in step 5 was maintained at 45-52 hours.

The temperature reduction time in the step 7 is maintained for 90 hours, and the temperature range is 1800-2200 ℃.

The working principle is as follows: in the invention, in the process of preparing the crystal, firstly, raw materials in a supply box 5 are added into a crucible 3 through a first guide pipe 601 and a second guide pipe 602 which are sucked by a booster pump 6, then the crucible 3 is sealed, inert gases such as helium and the like are input through an air inlet pipe 301 after vacuum pumping, the chemical reaction at high temperature is reduced, then a controller 101 is utilized to electrify a male electrode support leg and a female electrode support leg 401, a heating sleeve 4 is utilized to heat the crucible 3 to melt the raw materials in the crucible, the contact area between the heating sleeve 4 and the crucible 3 is reduced by utilizing a W-shaped through groove 402 at the position, thereby effectively adjusting and controlling the heating sequence and the cooling gradient of the crucible 3, the bottom wall of the crucible 3 is thinner than the top wall, the temperature is firstly lost from the bottom in the crystallization process of the crystal, the crystallization of the seed crystal can be sequentially crystallized, the formation of the crystal is ensured, and the redundant partial stress of a subsequently extracted crystal block, after the subsequent crystallization is finished, discharging gas in the crucible 3, opening the crucible 3, starting the electric telescopic rod 2 to send the heat conduction ring 202 into the crucible 3, heating the heat conduction ring 202 by the heater 201, raising the temperature of crystal around the crystal block by using the heat conduction ring 202, further reducing the stress connection between the crystal block and the unformed melt, preventing the crystal block from generating overlarge thermal shock when being separated, and ensuring the sequence integrity of the interior of the extracted crystal block.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.