CN115161771B - Method for self-supplying liquid gallium - Google Patents
Method for self-supplying liquid gallium Download PDFInfo
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- CN115161771B CN115161771B CN202210780215.4A CN202210780215A CN115161771B CN 115161771 B CN115161771 B CN 115161771B CN 202210780215 A CN202210780215 A CN 202210780215A CN 115161771 B CN115161771 B CN 115161771B
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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-replenishing liquid gallium. The invention sets a liquid gallium self-supplying device in the reaction cavity resource area to provide stable gallium liquid flow for the gallium boat. The liquid gallium self-replenishing device is provided with a high-temperature area, a low-temperature area and an intermediate area between the high-temperature area and the low-temperature area, wherein the intermediate area is filled with inert gas, heat is provided by the high-temperature area, the inert gas is heated and expanded, and pressure difference is generated after the gas is expanded, and the low-temperature area moves downwards at a constant speed, so that the liquid gallium is pushed to flow out stably. The condition that the yield of the monocrystalline GaN thick film substrate is affected due to the fact that the liquid level of the gallium liquid is reduced due to the chemical reaction of the gallium liquid in the gallium boat and HCl when the monocrystalline GaN thick film substrate is prepared by adopting an HVPE method in the prior art is avoided.
Description
Technical Field
The invention relates to the field of semiconductors, in particular to a method for self-replenishing liquid gallium.
Background
GaN is an important wide bandgap semiconductor material widely used for the preparation of high brightness LEDs, semiconductor lasers and high power electronics. Currently, a hydride vapor phase epitaxy (hydride vapor phase epitaxy, HVPE) method is mainly used to prepare a GaN single crystal thick film substrate. The method is usually carried out in a normal pressure thermal quartz reactor, and the basic chemical reaction is that gaseous HCl and liquid metal Ga are subjected to chemical reaction under a low-temperature environment to generate gaseous GaCl, and the GaCl is further reacted with NH 3 The reaction is carried out in a high-temperature environment to generate a GaN film, and reaction byproducts HCl and H 2 Can be recovered in a gaseous form. The HVPE preparation of gallium nitride requires two chemical reactions, i.e., a low temperature reaction and a high temperature reaction, so that the HVPE reactor needs to divide the reaction chamber into a low temperature region and a high temperature region, and many parameters need to be adjusted in the process to realize the controllable and deposition of the gallium nitride film.
At GaCl and NH 3 When the reaction occurs in a high-temperature environment, a stable GaCl source is a necessary condition for preparing a good GaN film, and in the process of generating gaseous GaCl by the chemical reaction of gaseous HCl and liquid metal Ga in a low-temperature environment, 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 of the generated GaCl cannot be kept stable due to the influence of factors such as surface tension and the like on the contact surface due to the fluctuation of the height of the contact surface.
Disclosure of Invention
The invention aims to provide a method for keeping the liquid level of a gallium boat.
In order to solve the technical problems, the invention provides a method for self-replenishing liquid gallium.
The liquid gallium self-replenishing device comprises:
the working area is a hollow column which is sealed up and down, and the working area is sequentially provided with:
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 middle 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 reaction cavity resource area; the temperature of the high temperature zone is higher than the temperature of the low temperature zone;
the gallium liquid reserving area is positioned at the lowest part in the working area and is used for containing gallium liquid, and openings are formed in two sides of the gallium liquid reserving area;
the gallium mouth is connected with an opening at one side of the gallium liquid reserved area;
when the gallium liquid discharging device works, because of the temperature difference between the high temperature area and the low temperature area, the inert gas in the middle area is heated and expanded to push the low temperature area to move downwards, so that the gallium liquid in the gallium liquid reserving area is discharged outwards through the gallium nozzle.
As a further improvement of the invention, the liquid gallium self-replenishing device further 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 supplying.
As a further improvement of the invention, the liquid gallium self-replenishing device is arranged in the reaction cavity resource area.
As a further improvement of the present invention, the high temperature region is made of a blackbody radiation material with a heat radiation absorptivity close to 1.
As a further improvement of the present invention, the low temperature zone material may be: quartz, silica.
As a further improvement of the invention, 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 region and the low temperature region.
The method for self-replenishing liquid gallium is realized by using the liquid gallium self-replenishing device, and comprises the following specific steps:
s01: the heat absorption of the high temperature zone reaches a high temperature above 880 ℃, and the temperature of the low temperature zone is equal to the reaction temperature of the resource zone by 820-880 ℃;
s02: utilizing the temperature difference between the high temperature zone and the low temperature zone, wherein the inert gas in the middle zone absorbs the heat of the high temperature zone and then expands after being heated;
s03: the inert gas after being heated and expanded generates pressure difference to automatically push the low-temperature area to move downwards;
s04: and 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 zone is realized by arranging an induction heater inside and designing an insulation layer outside.
As a further improvement of the invention, the independent high temperature of the high temperature zone is realized by absorbing the heat at the bottom of the resource zone by the blackbody material.
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 mouth and the height of the gallium mouth.
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 reaction cavity resource area to provide stable gallium liquid flow for a gallium boat. The liquid gallium self-replenishing device is provided with a high-temperature area, a low-temperature area and an intermediate area between the high-temperature area and the low-temperature area, wherein the intermediate area is filled with inert gas, heat is provided by the high-temperature area, the inert gas expands after being heated, and pressure difference is generated after the gas expands, the low-temperature area moves downwards at a uniform speed, so that the liquid gallium is pushed to flow out stably, the concentration fluctuation of GaCl generated due to the decrease of the liquid level of the gallium liquid is reduced, and the yield of the monocrystalline GaN thick film substrate is improved.
Drawings
Fig. 1 is a schematic diagram 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-replenishing device of the invention.
The reference numerals in the figures illustrate: 1. gallium boat, 2, substrate, 11, high temperature zone, 12, middle zone, 13, low temperature zone, 14, gallium liquid reserving zone, 15, gallium mouth, 16, gallium liquid storing zone, 17, gallium mouth inclination angle, 18, gallium mouth height.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
As described in the background section, in the prior art, a HVPE method is generally adopted to prepare a monocrystalline GaN thick film substrate, and in the preparation process, the liquid level of gallium liquid is reduced due to the chemical reaction of gallium liquid and HCl in a gallium boat, so that the growth rate and the crystal quality of the monocrystalline GaN thick film substrate are affected.
In order to solve the problem, the invention provides a method for self-replenishing liquid gallium, wherein a liquid gallium self-replenishing device is arranged in a reaction cavity resource area to provide stable gallium liquid flow for a gallium boat. The liquid gallium self-replenishing device is provided with a high-temperature area, a low-temperature area and an intermediate area between the high-temperature area and the low-temperature area, wherein the intermediate area is filled with inert gas, heat is provided by the high-temperature area, the inert gas expands after being heated, and the low-temperature area moves downwards at a constant speed due to pressure difference generated after the gas expands, so that the liquid gallium is pushed to stably flow out, and the liquid level of the gallium liquid in the gallium boat is maintained.
As shown in fig. 1, the reaction chamber in the HVPE apparatus includes a resource region where the gallium boat 1 is placed and a growth region where the substrate sheet 2 is placed. The temperature of the resource area is 820-880 ℃, and the resource area is used for the reaction of liquid gallium and HCl to generate GaCl; the temperature of the growth area is 1050 ℃, which is used for GaCl and NH 3 And (3) reacting to generate GaN crystals on the substrate sheet. Wherein multiple is arranged in the resource areaThe multiple gases are converged at the tail end of the resource region and react on the substrate slice 2 which is arranged in the concave growth region and parallel to the advancing direction of the gases to generate gallium nitride crystals.
The liquid gallium self-replenishing device structure is designed based on the method for self-replenishing liquid gallium, and is arranged in a reaction cavity resource area and is mainly used for providing stable liquid gallium flow for a gallium boat 1, so that the liquid level of a gallium source in the gallium boat 1 is controlled to be always in the optimal liquid level range of gallium required by a thick film substrate of monocrystalline GaN to be grown, and the optimal growth rate and crystal quality of nitride are ensured.
The structure of the liquid gallium self-replenishing device is schematically shown in fig. 2. Comprising the following steps:
the working area is a hollow column which is sealed up and down, and the working area is sequentially provided with:
the high temperature area 11 is a column with the same inner diameter as the working area, and is fixed at the upper end of the inside of the working area;
an intermediate zone 12, located below the high temperature zone 11, filled with an inert gas;
the low temperature region 13, the low temperature region 13 is a column with the same inner diameter as the working region, embedded in the working region and located below the middle region 12, and is made of common materials, such as: quartz, silicon oxide, etc., which is at the same temperature as the reaction temperature of the resource zone; the temperature of the high temperature zone is higher than the temperature of the low temperature zone;
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 14 is connected with the low-temperature area 13 and is provided with openings at two sides, 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;
a gallium mouth 15 connected with an opening on one side of the gallium liquid reserving region 14;
a gallium liquid storage area 16 connected to the other side opening of the gallium liquid reserving area 14, and storing a large amount of gallium liquid for supply therein;
when the gallium liquid storage device works, because of the temperature difference between the high-temperature region 11 and the low-temperature region 13, inert gas in the middle region 12 is heated and expanded to push the low-temperature region 13 to move downwards, so that gallium liquid in the gallium liquid reserving region 14 is discharged outwards through the gallium nozzle 15. Since the temperature difference is constant, the flow rate of the gallium liquid discharged from the gallium nozzle 15 is constant, and the effect of maintaining the liquid level in the gallium boat 1 is achieved. Since a large amount of gallium liquid is stored in the gallium liquid storage area 16, the gallium liquid reserving area 14 is connected with the gallium liquid storage area 16, and in one growth period (i.e. gallium nitride growth is completed once, gallium liquid is required to be cleaned in the gallium boat 1 after growth, and gallium liquid is required to be added in the gallium liquid storage area), the downward moving volume of the low temperature area 13 (the downward moving distance of the low temperature area multiplied by the cross-sectional area is the moving volume of the low temperature area) is equal to the volume of the discharged gallium liquid, and the discharged gallium liquid is enough for gallium liquid feeding in the gallium boat 1, so that the low temperature area 13 cannot move downward all the time in one growth period.
The design scheme of the inclination angle of the gallium nozzle 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 ) Is a volume difference, and this work is converted by internal energy e= (inR Δt)/2, where i is the degree of freedom, monatomic molecule is 3, diatomic molecule is 5, triatomic and polyatomic molecule 6; n is the amount of gaseous species; r is the ideal gas constant r=8.31J/K; Δt 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, alpha is the inclination angle 17 of the gallium mouth, and when alpha is 60 degrees, the pressure at the gallium mouth 15 is as follows: p=pgh=pghcos α, where H is the length of the gallium mouth 15, H is the height of the gallium mouth 15, and according to the calculation, the gallium mouth height 18 required to be designed is at most h=0.05m, so that the gallium liquid can be ensured to just flow out.
The pressure difference generated by the temperature difference is generated as soon as the reactor starts to grow GaN, and the minimum gallium nozzle inclination angle 17 and the maximum gallium nozzle 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 region 11 absorbs heat to reach a high temperature above 880 ℃, and the temperature of the low temperature region 13 is equal to the reaction temperature of the reaction cavity resource region 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 expands after being heated;
s03: the inert gas after being heated and expanded generates pressure difference to automatically push the low-temperature zone 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 of the gallium nozzle 15, so that stable liquid gallium flow is generated.
In an alternative embodiment, the pressure difference generated by the temperature difference can be regulated by adjusting the temperature of the high temperature region 11, and the flow rate of the gallium liquid can be adjusted in combination with the gallium nozzle inclination angle 17 and the gallium nozzle height 18.
Example 1
In an alternative embodiment, the high temperature region 11 of the liquid gallium self-replenishing device is made of the same material as the low temperature region 13, and the induction heater is arranged inside, so that the heat-insulating layer is designed outside to realize the high temperature exceeding 880 ℃.
Furthermore, the black body radiation material adopted in the high temperature area 11 is ZS-1061 high temperature resistant far infrared radiation energy-saving paint, and the paint is a novel energy-saving product specially developed for large combustion boiler industry, and enhances radiation heat exchange by utilizing the characteristics of high absorption, high heat storage, high heat release and high radiation of the black body material, so that the kiln efficiency is improved. When the temperature of the furnace body exceeds 800 ℃, heat is mainly transferred by radiation, and the radiation heat transfer is more than 15 times of convection and accounts for more than 80% of the total heat transfer. The high temperature radiation energy wavelength is mostly 1-15 mu m, for example, 78% and 88% of radiation energy is concentrated in the wave band when the temperature of the furnace body is 900 ℃ and 1300 ℃, the emissivity of common refractory materials in the wave band is very low, generally 0.6-0.8, the emissivity of the refractory materials can be reduced along with the rise of the furnace temperature, the emissivity of the ZS-1061 high temperature resistant far infrared radiation energy-saving coating can reach more than 0.92 at high temperature, the temperature of the furnace body can be controlled to be more than 960 ℃ when the temperature of a high temperature area is ensured to be more than 880 ℃, and the temperature of the furnace body can be selected to be more preferably between 1000 ℃ and 1050 ℃.
According to kirchhoff's law, the absorptivity and emissivity of a material are equal. When the emissivity of the surface of an object increases, its ability to absorb heat increases accordingly. Under the same heating condition, the heat transfer capability is improved, so that the heat utilization efficiency is improved greatly, and the purpose of energy conservation is achieved. ZS-1061 high-temperature-resistant far-infrared radiation energy-saving coating with high standard new technology adopts ZrO 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 electrons of the material 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-replenishing device adopts a blackbody radiation material with a heat radiation absorptivity close to 1, and the blackbody radiation material can completely absorb heat from the bottom of the reaction chamber to a high temperature above 880 ℃ and generate a temperature difference with the low temperature region 13.
The above-described embodiments are merely preferred embodiments for fully explaining the present invention, and the scope of the present invention is not limited thereto. Equivalent substitutions and modifications will occur to those skilled in the art based on the present invention, and are intended to be within the scope of the present invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. The utility model provides a liquid gallium is from replenishing device which characterized in that: comprising the following steps:
the working area is a hollow column which is sealed up and down, and the working area is sequentially provided with:
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 middle 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 reaction cavity resource area; the temperature of the high temperature zone is higher than the temperature of the low temperature zone;
the gallium liquid reserving area is positioned at the lowest part in the working area and is used for containing gallium liquid, and openings are formed in two sides of the gallium liquid reserving area;
the gallium mouth is connected with an opening at one side of the gallium liquid reserved area and is provided with an inclination angle;
when the gallium liquid discharging device works, because of the temperature difference between the high temperature area and the low temperature area, the inert gas in the middle area is heated and expanded to push the low temperature area to move downwards, so that the gallium liquid in the gallium liquid reserving area is discharged outwards through the gallium nozzle.
2. The liquid gallium self-replenishing device according to claim 1, wherein: the liquid gallium self-replenishing device further comprises a gallium liquid storage area which is connected with the opening at the other side of the gallium liquid reserved area, and a large amount of gallium liquid for supplying is stored in the liquid gallium self-replenishing device.
3. The liquid gallium self-replenishing device according to claim 1, wherein: the liquid gallium self-replenishing device is arranged in the reaction cavity resource area.
4. The liquid gallium self-replenishing device according to claim 1, wherein: the high temperature area adopts a blackbody radiation material with the heat radiation absorptivity close to 1.
5. The liquid gallium self-replenishing device according to claim 1, wherein: the low temperature area is made of the following materials: quartz, silica.
6. The liquid gallium self-replenishing device 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 intensity generated by the temperature difference of the high temperature area and the low temperature area.
7. A method for self-replenishing liquid gallium, characterized by: the liquid gallium self-replenishing device according to claims 1-6 comprises the following specific steps:
s01: the heat absorption of the high temperature zone reaches a high temperature above 880 ℃, and the temperature of the low temperature zone is equal to the reaction temperature of the resource zone by 820-880 ℃;
s02: utilizing the temperature difference between the high temperature zone and the low temperature zone, wherein the inert gas in the middle zone absorbs the heat of the high temperature zone and then expands after being heated;
s03: the inert gas after being heated and expanded generates pressure difference to automatically push the low-temperature area to move downwards;
s04: and 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 liquid gallium 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 preservation layer outside.
9. The method of self-replenishing liquid gallium according to claim 7, wherein: the independent high temperature of the high temperature area is realized by absorbing the heat at the bottom of the resource area through the blackbody material.
10. The method of self-replenishing liquid gallium according to claim 7, wherein: the flow rate of the gallium liquid is regulated by the pressure difference, the inclination angle of the gallium mouth and the height of the gallium mouth.
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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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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
-
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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| CN115161771A (en) | 2022-10-11 |
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