CN115161771A - Method for self-supplying gallium liquid - Google Patents
Method for self-supplying gallium liquid Download PDFInfo
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- CN115161771A CN115161771A CN202210780215.4A CN202210780215A CN115161771A CN 115161771 A CN115161771 A CN 115161771A CN 202210780215 A CN202210780215 A CN 202210780215A CN 115161771 A CN115161771 A CN 115161771A
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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
- 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
- C30B29/406—Gallium nitride
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
Abstract
The invention discloses a method for self-supplying liquid gallium. The invention arranges a liquid gallium self-supply device in the resource area of the reaction cavity to provide stable gallium liquid flow for the gallium boat. A high-temperature area, a low-temperature area and an intermediate area filled with inert gas and arranged between the high-temperature area and the low-temperature area are designed in the liquid gallium self-supply device, heat is provided through the high-temperature area, the inert gas is heated and expanded, pressure difference is generated after the gas is expanded, and the low-temperature area moves downwards at a constant speed, so that liquid gallium is pushed to flow out stably. The situation that the liquid level of gallium liquid is reduced due to the chemical reaction of the gallium liquid in the gallium boat and HCl when the monocrystal GaN thick film substrate is prepared by adopting an HVPE method in the prior art, so that the yield of the monocrystal GaN thick film substrate is influenced is avoided.
Description
Technical Field
The invention relates to the field of semiconductors, in particular to a method for automatically supplying gallium liquid.
Background
GaN is an important wide bandgap semiconductor material and is widely used for preparing high-brightness LEDs, semiconductor lasers and high-power electronic devices. At present, a GaN single crystal thick film substrate is mainly prepared by a Hydride Vapor Phase Epitaxy (HVPE) method. The method is generally carried out in a normal-pressure hot quartz reactor, and the basic chemical reaction is that gaseous HCl and liquid metal Ga are subjected to chemical reaction in a low-temperature environment to generate gaseous GaCl, and the GaCl is further subjected to chemical reaction to generate gaseous GaClAnd NH 3 Reacting at high temperature to generate GaN film and reaction by-products HCl and H 2 Can be recovered in a gaseous form. The HVPE for preparing the gallium nitride needs two chemical reactions, namely a low-temperature reaction and a high-temperature reaction, so that the HVPE reactor needs to divide a reaction chamber into a low-temperature area and a high-temperature area, and simultaneously, a plurality of parameters need to be adjusted in the process to realize the controllable and deposition of the gallium nitride film.
In GaCl and NH 3 When the reaction is carried out in a high-temperature environment, a stable GaCl source is a necessary condition for preparing a good GaN film, and in the process of carrying out chemical reaction on gaseous HCl and liquid metal Ga in a low-temperature environment to generate gaseous GaCl, the liquid level of the liquid metal Ga in a gallium boat continuously drops due to continuous consumption of the chemical reaction, and the output quantity of the generated GaCl cannot be kept stable due to the influence of factors such as surface tension and the like due to the height fluctuation of a contact surface.
Disclosure of Invention
The invention aims to provide a method capable of keeping the liquid level of a gallium boat.
In order to solve the technical problem, the invention provides a method for self-supplying liquid gallium.
The liquid gallium self-supply device comprises:
the workspace is a hollow column which is sealed from top to bottom, and is provided with the following components in sequence:
the high-temperature area is a column with the same inner diameter as the working area and is fixed at the upper end inside the working area;
the intermediate zone is positioned below the high-temperature zone and filled with inert gas;
the low-temperature area is a column with the same inner diameter as the working area, is embedded in the working area and is positioned below the middle area, and the temperature of the low-temperature area is equal to the reaction temperature in the resource area of the reaction cavity; the temperature of the high-temperature area is higher than that of the low-temperature area;
the gallium liquid reserving area is positioned at the lowest part in the working area, contains gallium liquid and is provided with openings at two sides;
the gallium mouth is connected with an opening on one side of the gallium liquid reserved area;
when the gallium liquid injection device works, due to the fact that the temperature difference exists between the high-temperature area and the low-temperature area, the inert gas in the middle area is heated and expanded, the low-temperature area is pushed to move downwards, and gallium liquid in the gallium liquid reserved area is discharged outwards through the gallium nozzle.
As a further improvement of the invention, the liquid gallium self-supply device also comprises a gallium liquid storage region which is connected with the opening at the other side of the gallium liquid reserved region and internally stores a large amount of gallium liquid for supply.
As a further improvement of the invention, the liquid gallium self-supply device is arranged in the resource region of the reaction cavity.
As a further improvement of the invention, the high-temperature region is made of black body radiation material with the thermal radiation absorptivity close to 1.
As a further improvement of the present invention, the material of the low temperature region may be: quartz, silicon oxide.
As a further improvement of the invention, the minimum inclination angle of the gallium nozzle and the maximum height of the gallium nozzle are determined by the pressure generated by the temperature difference of the high-temperature area and the low-temperature area.
The method for self-supplying the liquid gallium is realized by utilizing the liquid gallium self-supplying device, and comprises the following specific steps:
s01: the high-temperature area absorbs heat to reach a high temperature above 880 ℃, and the temperature of the low-temperature area and the reaction temperature of the resource area are kept equal to 820-880 ℃;
s02: the inert gas in the middle area absorbs the heat of the high-temperature area and then is heated and expanded by utilizing the temperature difference between the high-temperature area and the low-temperature area;
s03: the inert gas after being heated and expanded generates pressure difference to automatically push the low-temperature area to move downwards;
s04: the gallium liquid in the gallium liquid reserved area is extruded by the low-temperature area and flows out of the gallium nozzle, so that stable liquid gallium flow is generated.
As a further improvement of the invention, the independent high temperature of the high temperature area is realized by arranging an induction heater inside and designing an insulating layer outside.
As a further improvement of the invention, the independent high temperature of the high-temperature area is realized by absorbing the heat at the bottom of the resource area by black body materials.
As a further improvement of the invention, the flow rate of the gallium liquid is regulated by the pressure difference, the inclination angle of the gallium nozzle and the height of the gallium nozzle.
The invention has the beneficial effects that: the invention provides a method for self-supplying liquid gallium, which is characterized in that a liquid gallium self-supplying device is arranged in a resource region of a reaction cavity body to provide stable gallium liquid flow for a gallium boat. A high-temperature area, a low-temperature area and an intermediate area filled with inert gas and arranged between the high-temperature area and the low-temperature area are designed in the liquid gallium self-supply device, heat is provided through the high-temperature area, the inert gas is heated and expanded, pressure difference is generated after the gas is expanded, the low-temperature area moves downwards at a constant speed, and therefore liquid gallium is pushed to flow out stably, gaCl generation concentration fluctuation caused by the reduction of the liquid level of gallium liquid is reduced, and the yield of the single crystal GaN thick film substrate is improved.
Drawings
FIG. 1 is a schematic view of a reaction chamber in an HVPE apparatus of the invention.
FIG. 2 is a schematic diagram of the structure of the liquid gallium self-replenishment device of the present invention.
The reference numbers in the figures illustrate: 1. the gallium boat comprises a gallium boat body, 2 parts of a substrate, 11 parts of a high-temperature area, 12 parts of a middle area, 13 parts of a low-temperature area, 14 parts of a gallium liquid reserved area, 15 parts of a gallium nozzle, 16 parts of a gallium liquid storage area, 17 parts of a gallium nozzle inclination angle, 18 parts of a gallium nozzle height.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
As described in the background section, in the prior art, the HVPE method is usually adopted to prepare the single crystal GaN thick film substrate, and in the preparation process, the liquid level of the gallium liquid is reduced due to the chemical reaction of the gallium liquid in the gallium boat and the HCl, so that the growth rate and the crystal quality of the single crystal GaN thick film substrate are influenced.
Aiming at the problem, the invention provides a method for self-supplying liquid gallium, which is characterized in that a liquid gallium self-supplying device is arranged in a resource region of a reaction cavity body to provide stable gallium liquid flow for a gallium boat. A high-temperature area, a low-temperature area and an intermediate area filled with inert gas and arranged between the high-temperature area and the low-temperature area are designed in the liquid gallium self-supply device, heat is provided through the high-temperature area, the inert gas is heated and expanded, pressure difference is generated after the gas is expanded, the low-temperature area moves downwards at a constant speed, and therefore liquid gallium is pushed to flow out stably, and the liquid level height of gallium liquid in a gallium boat is maintained.
As shown in FIG. 1, the reaction chamber of the HVPE apparatus includes a source region in which a gallium boat 1 is placed and a growth region in which a substrate wafer 2 is placed. The temperature of the resource area is 820-880 ℃, and the resource area is used for reacting liquid gallium with HCl to generate GaCl; the temperature of the growth zone is 1050 ℃ for GaCl and NH 3 And reacting to generate GaN crystal on the substrate sheet. Wherein, the resource zone is provided with a plurality of channels for different gases to pass through, and a plurality of gases are converged at the tail end of the resource zone and react on the substrate slice 2 which is arranged in the concave growth zone and is parallel to the advancing direction of the gases to generate gallium nitride crystals.
The liquid gallium self-supply device is arranged in a resource region of a reaction cavity and is mainly used for providing stable liquid gallium flow for a gallium boat 1, so that the liquid level height of a gallium source in the gallium boat 1 is controlled to be always within the optimal liquid level height range of gallium liquid required by a substrate with a monocrystal GaN thick film to be grown, and the optimal growth rate and the crystal quality of nitride are ensured.
As shown in FIG. 2, the structure of the liquid gallium self-replenishment device is schematically shown. The method comprises the following steps:
the workspace is a hollow column which is sealed from top to bottom, and is provided with the following components in sequence from top to bottom:
the high-temperature area 11 is a column with the same inner diameter as the working area, and is fixed at the upper end inside the working area;
an intermediate zone 12 located below the high temperature zone 11 and filled with an inert gas;
the gallium liquid reserving area 14 is positioned at the lowest part in the working area, the upper part of the gallium liquid reserving area is connected with the low-temperature area 13, the gallium liquid is contained, openings are arranged at two sides of the gallium liquid reserving area, and when the gallium liquid reserving area 14 works, the gallium liquid in the gallium liquid reserving area 14 is pushed downwards by the low-temperature area 13 and is discharged outwards by the gallium liquid reserving area 14;
the gallium mouth 15 is connected with an opening at one side of the gallium liquid reserved area 14;
a gallium liquid storage region 16 connected with the other side opening of the gallium liquid reservation region 14, and a large amount of gallium liquid for supply is stored in the gallium liquid storage region;
when the gallium liquid distributor works, due to the temperature difference between the high-temperature area 11 and the low-temperature area 13, the inert gas in the middle area 12 is heated and expanded, the low-temperature area 13 is pushed to move downwards, and the gallium liquid in the gallium liquid reserving area 14 is discharged outwards through the gallium nozzle 15. Because the temperature difference is constant, the flow of the gallium liquid discharged by the gallium nozzle 15 is constant, thereby achieving the effect of maintaining the height of the liquid level in the gallium boat 1. Because a large amount of gallium liquid is stored in the gallium liquid storage region 16, the gallium liquid reservation region 14 is connected with the gallium liquid storage region 16, the volume of downward movement of the low-temperature region 13 (the downward movement distance of the low-temperature region multiplied by the sectional area is the volume of movement of the low-temperature region) is equal to the volume of the discharged gallium liquid in a growth cycle (namely, the growth of gallium nitride is completed once, the inside of the gallium boat 1 needs to be cleaned after the growth, and the gallium liquid is added into the gallium liquid storage region), and the discharged gallium liquid is enough for supplying the gallium liquid in the gallium boat 1, so in a growth cycle, the low-temperature region 13 cannot move downward all the time.
The design scheme of the inclination angle of the gallium mouth 15 is as follows: the gas expansion work is as follows: w = P (V) 2 -V 1 ) Wherein W is work, P is pressure, (V) 2 -V 1 ) For volume difference, this work is converted by internal energy E = (inR Δ T)/2, where i is the degree of freedom, monoatomic is 3, diatomic is 5, triatomic and polyatomic is 6; n is the amount of material of the gas; r is the ideal gas constant R =8.31J/K; Δ T is the temperature difference.Considering that the absorption rate of the blackbody radiation material is about 0.92 and energy loss exists in the energy absorption process, α is the gallium mouth inclination angle 17, and when α is 60 °, the pressure at the gallium mouth 15 is: p = ρ gh = ρ gHcos α, where H is the length of the gallium tip 15 and H is the height of the gallium tip 15, and the height 18 of the gallium tip to be designed is calculated to be H =0.05m at the maximum, so that the gallium liquid can be ensured to flow out just.
Wherein, as long as the reactor starts to grow GaN, the pressure difference generated by the temperature difference can be generated, and the minimum gallium mouth inclination angle 17 and the maximum gallium mouth height 18 when the gallium liquid just can flow out can be calculated through the pressure difference generated by the thermal expansion of the inert gas.
A method of self-replenishing liquid gallium comprising:
s01: the blackbody radiation material in the high-temperature zone 11 absorbs heat to reach a high temperature above 880 ℃, and the temperature of the low-temperature zone 13 and the reaction temperature of the reaction cavity resource zone are kept at 820-880 ℃;
s02: the intermediate zone 12 utilizes the temperature difference between the high temperature zone 11 and the low temperature zone 13, and the inert gas in the intermediate zone 12 absorbs the heat of the high temperature zone 11 and then is heated and expanded;
s03: the pressure difference generated by the heated and expanded inert gas automatically pushes the low-temperature area 13 to move downwards;
s04: the gallium liquid in the gallium liquid reserving area 14 is extruded by the low-temperature area 13 and flows out from the gallium mouth 15, thereby generating stable liquid gallium flow.
In an alternative embodiment, the pressure difference generated by the temperature difference can be adjusted by adjusting the temperature of the high temperature region 11, and the flow rate of the gallium liquid can be adjusted by combining the inclination angle 17 of the gallium nozzle and the height 18 of the gallium nozzle.
Example 1
In an alternative embodiment, the high-temperature zone 11 of the liquid gallium self-supply device is made of the same material as the low-temperature zone 13, an induction heater is arranged inside the high-temperature zone, and an insulating layer is designed outside the high-temperature zone to realize the high temperature of more than 880 ℃.
Furthermore, the blackbody radiation material adopted in the high-temperature zone 11 is ZS-1061 high-temperature resistant far infrared radiation energy-saving coating which is a novel energy-saving product specially developed for the large-scale combustion boiler industry, and the characteristics of high absorption, high heat storage, high heat release and high radiation of the blackbody material are utilized to strengthen radiation heat exchange and improve the efficiency of the furnace. Generally, when the temperature of the furnace body exceeds 800 ℃, heat is mainly transferred by radiation, the radiation heat transfer is more than 15 times of convection, and accounts for more than 80% of the total heat transfer. The wavelength of high-temperature radiation energy is mostly 1-15 μm, for example, when the temperature of the furnace body is 900 ℃ and 1300 ℃, 78% and 88% of radiation energy are respectively concentrated in the wave band, the emissivity of common refractory materials in the wave band is very low, generally 0.6-0.8, the emissivity of the refractory materials is reduced along with the rise of the furnace temperature, the emissivity is only 0.4-0.6 at high temperature, while the emissivity of the ZS-1061 high-temperature far infrared radiation resistant energy-saving coating can reach above 0.92, when the temperature of a high-temperature zone is ensured to be above 880 ℃, the temperature of the furnace body can be controlled to be above 960 ℃, and more preferably, the temperature of the furnace body can be selected to be between 1000-1050 ℃.
According to kirchhoff's law, the absorptivity and emissivity of a material are equal. When the emissivity of the surface of the object is increased, the capacity of the surface of the object to absorb heat is correspondingly increased. Under the condition of high temperature, the heat transfer is mainly radiation, after the surface of the heated object is coated with a nano-micron high-radiation coating, the capacity of the heated object for absorbing and emitting heat is greatly improved, and under the same heating condition, the utilization efficiency of heat energy is certainly greatly improved due to the improvement of the heat transfer capacity, so that the aim of saving energy is fulfilled. ZrO is adopted as high-standard new technology ZS-1061 high-temperature-resistant far infrared radiation energy-saving coating 2 、BN、SiC、MgO、La 2 O 3 、MnO 2 、Cr 2 O 3 The refractory materials such as BeO, silicate and the like are doped at high temperature to form solid solution, so that the energy level of material electrons is increased, the infrared radiation coefficient of heat energy is improved, the corresponding good performances such as heat resistance, high strength, corrosion resistance, wear resistance and the like are maintained, and the energy-saving effect of the coating is improved.
In an alternative embodiment, the high temperature region 11 of the liquid gallium self-supplying device is made of blackbody radiation material with a thermal radiation absorption rate close to 1, and the blackbody radiation material can completely absorb heat from the bottom of the reaction chamber to reach a high temperature above 880 ℃, and generate a temperature difference with the low temperature region 13.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. A liquid gallium self-supply device is characterized in that: the method comprises the following steps:
the workspace is a hollow column which is sealed from top to bottom, and is provided with the following components in sequence from top to bottom:
the high-temperature area is a column with the same inner diameter as the working area and is fixed at the upper end inside the working area;
the intermediate zone is positioned below the high-temperature zone and filled with inert gas;
the low-temperature area is a column with the same inner diameter as the working area, is embedded in the working area and is positioned below the middle area, and the temperature of the low-temperature area is equal to the reaction temperature in the resource area of the reaction cavity; the temperature of the high-temperature area is higher than that of the low-temperature area;
the gallium liquid reserving area is positioned at the lowest part in the working area, contains gallium liquid and is provided with openings at two sides; the gallium nozzle is connected with an opening on one side of the gallium liquid reserved area;
when the gallium liquid injection device works, due to the fact that the temperature difference exists between the high-temperature area and the low-temperature area, the inert gas in the middle area is heated and expanded, the low-temperature area is pushed to move downwards, and gallium liquid in the gallium liquid reserved area is discharged outwards through the gallium nozzle.
2. The liquid gallium self-replenishment device according to claim 1, wherein: the liquid gallium self-supply device also comprises a gallium liquid storage area which is connected with the opening at the other side of the gallium liquid reserved area and internally stores a large amount of gallium liquid for supply.
3. The liquid gallium self-replenishment device according to claim 1, wherein: the liquid gallium self-supply device is arranged in the reaction cavity resource area.
4. The liquid gallium self-replenishment apparatus according to claim 1, wherein: the high-temperature area adopts black body radiation material with the thermal radiation absorption rate close to 1.
5. The liquid gallium self-replenishment apparatus according to claim 1, wherein: the low temperature zone material can be: quartz, silicon oxide.
6. The liquid gallium self-replenishment apparatus according to claim 1, wherein: the minimum inclination angle of the gallium mouth and the maximum height of the gallium mouth are determined by the pressure generated by the temperature difference of the high-temperature area and the low-temperature area.
7. A method for self-replenishing liquid gallium, comprising: the liquid gallium self-supplying device is realized by the liquid gallium self-supplying device of claims 1 to 6, and comprises the following specific steps:
s01: the high-temperature area absorbs heat to reach a high temperature above 880 ℃, and the temperature of the low-temperature area and the reaction temperature of the resource area are kept equal to 820-880 ℃;
s02: the inert gas in the middle area absorbs the heat of the high-temperature area and then is heated and expanded by utilizing the temperature difference between the high-temperature area and the low-temperature area;
s03: the inert gas after being heated and expanded generates pressure difference to automatically push the low-temperature area to move downwards;
s04: the gallium liquid in the gallium liquid reserved area is extruded by the low-temperature area and flows out of the gallium nozzle, so that stable liquid gallium flow is generated.
8. The method of self-replenishing gallium from liquid according to claim 7, wherein: the independent high temperature of the high temperature area is realized by arranging an induction heater inside and designing a heat insulation layer outside.
9. The method of self-replenishing gallium from liquid according to claim 7, wherein: the independent high temperature of high temperature region is realized through black body material absorption resource district bottom heat.
10. The method of self-replenishing gallium from liquid according to claim 7, wherein: the flow rate of the gallium liquid is regulated by the pressure difference, the inclination angle of the gallium nozzle and the height of the gallium nozzle.
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| CN202210780215.4A CN115161771B (en) | 2022-07-04 | 2022-07-04 | Method for self-supplying liquid gallium |
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| CN202210780215.4A CN115161771B (en) | 2022-07-04 | 2022-07-04 | Method for self-supplying liquid gallium |
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| CN2585160Y (en) * | 2002-10-28 | 2003-11-05 | 顾安胜 | High-temp. heat exchanger |
| CN202376965U (en) * | 2011-11-27 | 2012-08-15 | 陈晓容 | Microfeeding device based on steam medium |
| CN103122835A (en) * | 2013-01-10 | 2013-05-29 | 杨健飞 | Temperature difference engine |
| CN105986313A (en) * | 2015-01-31 | 2016-10-05 | 东莞市中镓半导体科技有限公司 | Gallium source automatic supply and recovery device |
| CN212735261U (en) * | 2020-08-26 | 2021-03-19 | 黄小离 | Automatic lubricating cooling liquid supply device |
| CN114108097A (en) * | 2021-11-10 | 2022-03-01 | 南通大学 | Device and method for improving growth uniformity of gallium nitride crystal |
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2022
- 2022-07-04 CN CN202210780215.4A patent/CN115161771B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2585160Y (en) * | 2002-10-28 | 2003-11-05 | 顾安胜 | High-temp. heat exchanger |
| CN202376965U (en) * | 2011-11-27 | 2012-08-15 | 陈晓容 | Microfeeding device based on steam medium |
| CN103122835A (en) * | 2013-01-10 | 2013-05-29 | 杨健飞 | Temperature difference engine |
| CN105986313A (en) * | 2015-01-31 | 2016-10-05 | 东莞市中镓半导体科技有限公司 | Gallium source automatic supply and recovery device |
| CN212735261U (en) * | 2020-08-26 | 2021-03-19 | 黄小离 | Automatic lubricating cooling liquid supply device |
| CN114108097A (en) * | 2021-11-10 | 2022-03-01 | 南通大学 | Device and method for improving growth uniformity of gallium nitride crystal |
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