CN113061981A - Thermal field structure for sapphire crystal growth and growth method thereof - Google Patents

Thermal field structure for sapphire crystal growth and growth method thereof Download PDF

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Publication number
CN113061981A
CN113061981A CN202110271473.5A CN202110271473A CN113061981A CN 113061981 A CN113061981 A CN 113061981A CN 202110271473 A CN202110271473 A CN 202110271473A CN 113061981 A CN113061981 A CN 113061981A
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heater
crystal
temperature
power
growth
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欧阳鹏根
张俊
曹建伟
石刚
宋建军
付春雷
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Inner Mongolia Jinghuan Electronic Materials Co ltd
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Inner Mongolia Jinghuan Electronic Materials Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/14—Heating of the melt or the crystallised materials
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/20—Aluminium oxides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/02—Heat treatment

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a sapphire crystal growth thermal field structure and a growth method thereof. The in-situ annealing in the growth method comprises the following steps: the power of the side heater and the power of the bottom heater are respectively and slowly reduced, and the power of the top heater is slowly increased until the temperature measured by the top temperature measuring unit reaches 1900 ℃, and the temperature reduction process is reduced by no more than 20 ℃/hr; maintaining the power of the top heater, the side heater and the bottom heater for 20 hr; the top heater, the side heater and the bottom heater respectively and slowly reduce the power until the temperature measured by the top temperature measuring unit reaches 1000 ℃, and the temperature reduction process does not fall by more than 20 ℃/hr; maintaining the power of the top heater, the side heater and the bottom heater for 20 hr; the top heater, the side heater and the bottom heater respectively and slowly reduce the power to zero, the temperature is cooled to the normal temperature of the crystal, and the temperature reduction process is reduced by no more than 30 ℃/hr.

Description

Thermal field structure for sapphire crystal growth and growth method thereof
Technical Field
The invention relates to the field of crystal growth and manufacturing, in particular to a sapphire crystal growth thermal field structure and a growth method thereof.
Background
Sapphire crystal is an important basic material in modern industry, sapphire has high strength, high hardness and scouring resistance, and is widely applied to infrared window devices, satellite space technology and high-strength laser window materials. The unique lattice structure, excellent mechanical property and good thermal property of the sapphire crystal enable the sapphire crystal to become the most ideal substrate material for semiconductor GaN/Al2O3 Light Emitting Diodes (LEDs), large-scale integrated circuit SOI and SOS, superconducting nano-structure films and the like in practical application. With the requirement of a special optical window on larger size and lower residual stress of a sapphire material, the development of sapphire crystals with the weight of more than 300kg, particularly ultra-large sapphire crystals with the weight of 600kg-700kg, is of urgent significance. But 600kg-700kg of oversized sapphire crystal faces bottlenecks of crystal cracking, large residual stress and the like. Sapphire crystal growth needs to form a certain temperature gradient in a melt and a crystal so as to ensure the formation of a driving force for crystal growth, but meanwhile, the temperature difference can form thermal stress in the crystal, so that the subsequent processing of a sapphire product is adversely affected, and the sapphire product generally needs to be re-annealed. When the residual thermal stress is larger than the allowable stress of the sapphire crystal, the crystal cracking is also caused, and the crystal cracking is one of the technical bottlenecks of the large-size sapphire crystal as the size of the sapphire crystal is increased more obviously.
At present, the traditional sapphire crystal is still within 200kg, the diameter is generally not more than 350mm, the height is not more than 400mm, the temperature difference of the sapphire crystal in a thermal field is not too large, the traditional heater configuration or the staged annealing can meet the requirements, and more documents and patents are published. However, the diameter of the 600kg-700 kg-grade sapphire crystal exceeds 550mm, the height of the sapphire crystal exceeds 700mm, the latent heat of the sapphire crystal is large, the temperature difference is large, the problems that the sapphire crystal is easy to crack and has large residual stress in the annealing process at the high temperature of 2050 ℃ are caused, and the requirements cannot be met by adopting the traditional heater structure and the annealing process. Therefore, the development of a thermal field structure suitable for 600kg-700kg of ultra-large sapphire crystals and a corresponding crystal in-situ annealing process have very urgent significance, and a foundation is laid for the subsequent processing of high-quality large-size panels.
Disclosure of Invention
The invention mainly aims to overcome the defects in the prior art and provides a thermal field structure for sapphire crystal growth and a crystal growth method. By the thermal field structure and the crystal growth method, the problems of annealing cracking and large residual stress of 600kg-700kg of ultra-large sapphire crystals can be solved, and a foundation is laid for subsequent processing of high-quality large-size panels.
In order to solve the technical problem, the solution of the invention is as follows:
the utility model provides a sapphire crystal growth thermal field structure, including crucible, seed rod, the heater that is used for holding the crystal and set up at the outlying heat retainer of heater, its characterized in that: heaters, namely a side heater, a top heater and a bottom heater are arranged at the side part, the top part and the bottom part of the crucible respectively, and the heaters can independently control power.
As an improvement, the temperature measuring device also comprises a top temperature measuring unit and a bottom temperature measuring unit which are respectively arranged at the top and the bottom of the heat insulating body.
As an improvement, the top temperature measuring unit and the bottom temperature measuring unit both adopt a bicolor infrared thermometer, and the temperature measuring range is 800-2500 ℃.
As an improvement, the top heater and the top of the heat preservation body are provided with temperature measuring channels, the bottom heater and the bottom of the heat preservation body are provided with temperature measuring channels, and the temperature measuring channels are used for the top temperature measuring unit and the bottom temperature measuring unit to measure the temperature of different parts of the crystal or the temperature of the crucible.
The invention also provides a growth method of the growth thermal field structure, which comprises the steps of preparation work, seeding, expanding growth, equal-diameter growth, crystal ending and in-situ annealing, and is characterized in that: the in-situ annealing steps and strategies include:
annealing stage 1: the power of the side heater and the power of the bottom heater are respectively and slowly reduced according to a certain amplitude, the power of the top heater is slowly increased according to a certain amplitude, so that the temperature of the crystal is slowly reduced until the temperature of the sapphire crystal measured by the top temperature measuring unit reaches 1900 ℃, and the temperature of the sapphire crystal is ensured to be reduced by no more than 20 ℃/hr in the cooling process;
and (2) annealing stage: keeping the power of the top heater, the side heater and the bottom heater unchanged for 20 hr;
and (3) annealing stage: the top heater, the side heater and the bottom heater respectively and slowly reduce power according to a certain range until the temperature of the crystal is up to 1000 ℃ displayed by the top temperature measuring unit, and the temperature of the sapphire crystal is ensured to be reduced by no more than 20 ℃/hr in the temperature reduction process;
and 4, annealing stage: keeping the power of the top heater, the side heater and the bottom heater unchanged for 20 hr;
and (5) annealing stage: the top heater, the side heater and the bottom heater are respectively and slowly reduced to zero according to a certain range, and are naturally cooled until the temperature of the crystal is reduced to normal temperature, and the temperature reduction range of the sapphire crystal is not more than 30 ℃/hr in the temperature reduction process.
In the step of the isometric growth, a top heater is used as an auxiliary heater, power is not applied in the crystal growth process, and the isometric growth of the crystal is completed by the output power of a side heater and a bottom heater; in the crystal ending step: after the crystal growth is finished, the crystal is pulled up through the seed rod, so that the crystal is completely separated from the liquid level and is about 50mm away from the bottom of the crucible.
As an improvement, during the in-situ annealing step, the power control strategies of the top heater, the side heaters and the bottom heater ensure that the temperature of the bottom temperature measurement unit is always higher than that of the top temperature measurement unit, but the temperature difference does not exceed 10 ℃.
As an improvement, the crystal is driven by the seed rod to rotate at a constant speed in the processes of crystal equal-diameter growth and in-situ annealing.
As an improvement, argon or nitrogen protective gas is introduced into the growth thermal field structure in the processes of crystal isodiametric growth and in-situ annealing.
In the invention, the side heater and the bottom heater are mainly used as main heaters in the equal-diameter growth process, and the top heater does not apply power and is only used as an auxiliary heater used in the annealing stage, so that the crystal has larger radial temperature gradient and axial temperature gradient in the crystal growth process, and the crystal growth keeps enough driving force. After the growth of the crystal is finished and the crystal enters an annealing process, the power of the top heater is gradually increased in the annealing stage 1, and the power of the side heater and the bottom heater is reduced, so that the axial and radial temperature gradients in the crystal are gradually reduced, and the temperature difference of the crystal in the annealing process is smaller through the auxiliary judgment of the top temperature measuring device (such as a top temperature measuring unit) and the bottom temperature measuring device (such as a bottom temperature measuring unit), so that the equal-temperature annealing of the crystal is realized.
Compared with the prior art, the invention has the following beneficial effects: during the growth of the crystal, proper power is applied through the side heater and the bottom heater to ensure that the crystal has enough axial and radial temperature gradients and enough driving force during the growth. In the annealing process, the crystal is annealed at the same temperature by starting the auxiliary heater-the top heater and adjusting the power properly, so that the problem that the 600kg-700kg oversized crystal is easy to crack is successfully solved. Meanwhile, the thermal stress of the crystal is small, so that a subsequent heavy annealing process of the large-size sapphire panel can be omitted, and the subsequent processing cost and the process difficulty are reduced.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Fig. 2 is a graph comparing the effect of the present invention on the radial and axial temperature of the crystal after annealing stage 1 of the prior art.
The reference numbers in the figures are: 1, a top temperature measuring unit; 2, a seed rod; 3 a top heater (referred to as "top heater"); 4, crystals; 5, a crucible; 6 side heaters (simply "side heaters"); 7 a bottom heater (simply "bottom heater"); 8, a heat insulator; and 9, a bottom temperature measuring unit.
Detailed Description
The invention is described in detail below with reference to the following figures and detailed description: the crucible comprises a crucible for containing crystals, a seed rod, a heater and a heat preservation body arranged on the periphery of the heater, wherein the heaters are arranged on the side part, the top part and the bottom part of the crucible, and are respectively a side heater, a top heater and a bottom heater, and the heaters can independently control power.
Specifically, as shown in fig. 1 and 2, the invention provides a thermal field structure for sapphire crystal growth, which mainly comprises a sapphire crystal 4 and a crucible 5, and also comprises a seed rod 2, a heater, a heat insulator 8 and a temperature measuring unit; the crystal 4 is placed at the lower end of the seed rod and is positioned in the crucible; the side part, the top part and the bottom part of the crucible are respectively provided with a heater, namely a side heater, a top heater and a bottom heater, which can independently control the power, wherein the top heater and the top part of the heat insulator are provided with temperature measuring channels, the bottom heater and the bottom of the heat insulator are provided with temperature measuring channels, and the temperature measuring channels are used for the top temperature measuring unit and the bottom temperature measuring unit to measure the temperature of different parts of the crystal or the crucible; the top temperature measuring unit 1 and the bottom temperature measuring unit 9 are respectively arranged at the top and the bottom of the heat insulation body.
In the invention, the top temperature measuring unit 1 and the bottom temperature measuring unit 9 are both two-color infrared thermometers, and the temperature measuring range is 800-2500 ℃.
The sapphire crystal growth method comprises the working procedures of preparation, seeding, expanding growth, isometric growth, crystal ending, in-situ annealing and the like.
In the invention, the method for constant diameter growth and in-situ annealing comprises the following steps:
(1) and (3) isometric growth: the top heater is used as an auxiliary heater to apply no power, the crystal growth is completed mainly by the power of the side heater and the bottom heater, larger radial and axial temperature gradients can be ensured in the crystal, and the crystal growth is ensured to have enough driving force;
(2) crystal ending: after the crystal growth is finished, pulling the crystal through a seed rod to ensure that the crystal is completely separated from the liquid level and is about 50mm away from the bottom of the crucible;
(3) annealing stage 1: the top heater slowly increases power according to a certain amplitude, the side heater and the bottom heater respectively slowly decrease power according to a certain amplitude, the temperature of the crystal is ensured to slowly decrease until the temperature of the sapphire crystal measured by the top temperature measuring unit reaches 1900 ℃, and the temperature of the sapphire crystal is ensured to decrease by no more than 20 ℃/hr in the temperature reduction process;
(4) and (2) annealing stage: keeping the power of the top heater, the side heater and the bottom heater constant for 20 hr;
(5) and (3) annealing stage: the top heater, the side heater and the bottom heater respectively and slowly reduce power according to a certain range until the temperature displayed by the top temperature measuring unit reaches 1000 ℃, and the temperature of the sapphire crystal is ensured to be reduced by less than 20 ℃/hr in the temperature reduction process;
(6) and 4, annealing stage: keeping the power of the top heater, the side heater and the bottom heater constant for 20 hr;
(7) and (5) annealing stage: the top heater, the side heater and the bottom heater respectively slowly reduce the power to zero according to a certain range, and naturally cool until the temperature of the crystal is reduced to normal temperature, and the temperature reduction range of the sapphire crystal is ensured not to exceed 30 ℃/hr in the temperature reduction process.
In the invention, the temperature difference of the bottom temperature measuring unit and the top temperature measuring unit in the in-situ annealing process of the crystal is ensured to be between 0 and 10 ℃ by controlling the power of the heaters properly. The specific different heater power control strategies can be obtained through limited experiments or finite element simulation techniques and other approaches according to temperature measurement data of different parts of the crystal.
In the invention, the crystal is driven by the seed crystal rod to rotate at a constant speed in the processes of equal-diameter growth and in-situ annealing so as to ensure the axial symmetry of the temperature distribution of the crystal.
In the invention, argon or nitrogen protective gas is introduced into the growth thermal field structure in the processes of equal-diameter growth and in-situ annealing.
As shown in fig. 2, which is a schematic diagram of radial temperature and axial temperature distribution in the conventional technical scheme and the technical scheme adopted in the crystal annealing process, it can be seen that in the crystal annealing stage 1, the axial temperature gradient and the radial temperature gradient of the crystal are reduced by increasing the power of the top heater and reducing the side heater and the bottom heater: the radial temperature difference of the crystal can be reduced to be within 10 ℃ from more than 40 ℃ in the traditional technical scheme, and the axial temperature difference of the crystal can be reduced to be within 10 ℃ from more than 60 ℃. The crystal is nearly isothermal at different locations during annealing, thereby reducing thermal stress generation of the crystal due to temperature differences. The technical scheme is adopted to successfully solve the problem that 600kg-700kg of oversized crystal is easy to crack, and 720kg of kyropoulos sapphire crystal is successfully grown.
The invention only refers to the temperature difference control of the top temperature measuring unit and the bottom temperature measuring unit as well as the temperature difference control of the top temperature and the bottom temperature of the crystal, and the radial temperature difference and the axial temperature difference of the crystal can be controlled by the arrangement of the temperature measuring units at different positions and the adjustment of the shape, the number and the position of the heater.
It is obvious that the present invention is not limited to the above embodiments, but many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.

Claims (9)

1. The utility model provides a sapphire crystal growth thermal field structure, is including crucible, seed rod, the heater that is used for holding the crystal and set up at heater outlying heat-preservation body, its characterized in that: heaters, namely a side heater, a top heater and a bottom heater are arranged at the side part, the top part and the bottom part of the crucible respectively, and the heaters can independently control power.
2. The growing thermal field structure of claim 1, wherein: the temperature measurement device also comprises a top temperature measurement unit and a bottom temperature measurement unit which are respectively arranged at the top and the bottom of the heat insulation body.
3. The growing thermal field structure of claim 2, wherein: the top temperature measuring unit and the bottom temperature measuring unit both adopt a bicolor infrared thermometer, and the temperature measuring range is 800-2500 ℃.
4. The growing thermal field structure of any one of claims 1-3, wherein: the top heater and the top of the heat insulator are provided with temperature measuring channels, the bottom heater and the bottom of the heat insulator are provided with temperature measuring channels, and the temperature measuring channels are used for the top temperature measuring unit and the bottom temperature measuring unit to measure the temperature of different parts of the crystal or the temperature of the crucible.
5. A method of growing a thermal field structure according to any one of claims 1 to 4, the method comprising preparation work-seeding-diameter expansion growth-isometric growth-crystal ending-in situ annealing, characterized in that: the in-situ annealing step comprises:
annealing stage 1: the power of the side heater and the power of the bottom heater are respectively and slowly reduced, and the power of the top heater is slowly increased, so that the temperature of the crystal is slowly reduced until the temperature of the sapphire crystal measured by the top temperature measuring unit reaches 1900 ℃, and the temperature of the sapphire crystal is ensured to be reduced by no more than 20 ℃/hr in the temperature reduction process;
and (2) annealing stage: keeping the power of the top heater, the side heater and the bottom heater unchanged for 20 hr;
and (3) annealing stage: the power of the top heater, the side heater and the bottom heater is respectively and slowly reduced until the temperature of the crystal is up to 1000 ℃ as shown by the top temperature measuring unit, and the temperature of the sapphire crystal is ensured to be reduced by no more than 20 ℃/hr in the cooling process;
and 4, annealing stage: keeping the power of the top heater, the side heater and the bottom heater unchanged for 20 hr;
and (5) annealing stage: the top heater, the side heater and the bottom heater respectively slowly reduce the power to zero, and naturally cool until the temperature of the crystal is reduced to normal temperature, and the temperature of the sapphire crystal is ensured to be reduced by no more than 30 ℃/hr in the cooling process.
6. The growing method according to claim 5, wherein: in the step of equal-diameter growth, the top heater is used as an auxiliary heater, power is not applied in the crystal growth process, and the equal-diameter growth of crystals is completed by the output power of the side heater and the bottom heater; in the crystal ending step: after the crystal growth is finished, the crystal is pulled up through the seed rod, so that the crystal is completely separated from the liquid level and is about 50mm away from the bottom of the crucible.
7. The growing method according to claim 5, wherein: in the in-situ annealing step process, the power control of the top heater, the side heater and the bottom heater ensures that the temperature of the bottom temperature measuring unit is always higher than that of the top temperature measuring unit, but the temperature difference does not exceed 10 ℃.
8. The growing method according to claim 5, wherein: the crystal is driven by the seed crystal rod to rotate at a constant speed in the processes of crystal isometric growth and in-situ annealing.
9. The growing method according to claim 5, wherein: and introducing argon or nitrogen protective gas into the growth thermal field structure in the processes of crystal isometric growth and in-situ annealing.
CN202110271473.5A 2021-03-12 2021-03-12 Thermal field structure for sapphire crystal growth and growth method thereof Pending CN113061981A (en)

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CN202110271473.5A CN113061981A (en) 2021-03-12 2021-03-12 Thermal field structure for sapphire crystal growth and growth method thereof

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