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WO2019222997A1 - Appareil et procédé de préparation d'un cristal de nitrure d'aluminium - Google Patents

Appareil et procédé de préparation d'un cristal de nitrure d'aluminium Download PDF

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Publication number
WO2019222997A1
WO2019222997A1 PCT/CN2018/088423 CN2018088423W WO2019222997A1 WO 2019222997 A1 WO2019222997 A1 WO 2019222997A1 CN 2018088423 W CN2018088423 W CN 2018088423W WO 2019222997 A1 WO2019222997 A1 WO 2019222997A1
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WO
WIPO (PCT)
Prior art keywords
crucible
diameter
aluminum nitride
substrate
raw material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2018/088423
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English (en)
Chinese (zh)
Inventor
覃佐燕
武红磊
钟旭辉
郑瑞生
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Shenzhen University
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Shenzhen University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenzhen University filed Critical Shenzhen University
Priority to PCT/CN2018/088423 priority Critical patent/WO2019222997A1/fr
Publication of WO2019222997A1 publication Critical patent/WO2019222997A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/02—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method without using solvents
    • 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
    • C30B29/38—Nitrides

Definitions

  • the invention belongs to the technical field of material preparation, and particularly relates to a device and method for preparing aluminum nitride crystals.
  • Deep ultraviolet light-emitting devices have a wide range of applications in sterilization, water purification, biomedicine, and deep ultraviolet light sources.
  • aluminum nitride crystals have high temperature and pressure resistance, extremely high piezoelectric effect, and high electron mobility. It has broad prospects in applications such as high-power electronic devices and is an ideal semiconductor material for the preparation of deep ultraviolet light-emitting devices.
  • the preparation of aluminum nitride crystal materials is difficult. At present, the research on aluminum nitride crystals at home and abroad still stays on the preparation size of the centimeter level.
  • the sublimation method also known as physical vapor transmission method
  • the sublimation method is considered to be the most promising method.
  • the aluminum nitride material sublimates in the high temperature region, and then re-evaluates in the low temperature region. Crystals form crystals.
  • the aluminum nitride single crystal prepared by this method has the following disadvantages: (1) Due to the strong anisotropy shown during the growth of aluminum nitride crystals, the nucleation rate of spontaneous nucleation of aluminum nitride in the early stage of growth is difficult. Got control. (2) Expand the size of aluminum nitride crystals. The seed crystal induction method currently used cannot find a suitable seed crystal, which is difficult to implement.
  • the following methods are mainly used at present.
  • One is the lateral gas transmission method.
  • the closed crucible structure with a conical shape at the end of the crucible (as the crystal selection area) is used to control the nucleation rate and grow a larger size
  • the crucible in this method cannot be used repeatedly, the cost is high, and the repeatability of the experiment is not high, resulting in poor quality of the aluminum nitride crystal.
  • tantalum carbide TiC
  • TiC tantalum carbide
  • the numerical simulation through this method can obtain the supersaturation range (0.25 ⁇ 0.3) suitable for crystal growth.
  • the content of carbon impurities in the crystals grown by this method is high, which affects the quality of the crystals. It is also difficult to obtain large-sized crystals, and the growth period is longer.
  • the other is a three-zone resistance heating inversion temperature field physical vapor transmission method to control nucleation.
  • the growth of aluminum nitride crystals is more random.
  • the nucleation is restricted by using a geometric structure by opening holes in the substrate The nucleation rate is better controlled, but it makes it difficult to expand the crystal in the later stage, which is not conducive to the growth of large-sized aluminum nitride single crystals.
  • the present invention provides an apparatus and method for preparing aluminum nitride crystals, which aims to solve the problems of high carbon impurity content, poor quality, difficulty in obtaining large-sized crystals, and long growth cycles in the existing aluminum nitride crystals.
  • An apparatus for preparing an aluminum nitride crystal includes: a first crucible, a second crucible, a substrate, and a temperature adjustment table;
  • the first crucible includes a raw material cavity and a reaction cavity, wherein the diameter of the reaction cavity is larger than the diameter of the raw material cavity, the raw material cavity is located at the bottom of the first crucible, and the reaction cavity is located at the first crucible. Opening
  • the substrate covers the opening of the first crucible, so that the aluminum nitride crystals are condensed on the substrate after the reaction chamber is sublimed;
  • the temperature adjustment platform is a hollow structure, and the side with the smallest diameter of the hollow part is placed on the substrate to adjust the contact area between the substrate and outside air;
  • the second crucible includes a raw material cavity and a reaction cavity, wherein the raw material cavity of the second crucible is located at the bottom of the second crucible, and the diameter of the raw material cavity of the second crucible is smaller than the reaction cavity of the second crucible. diameter of.
  • the invention provides a method for preparing an aluminum nitride crystal, including:
  • the diameter of the hollow part of the temperature adjustment table is increased, and the temperature is increased to 400 ° C to 600 ° C / h to 1900 ° C to 2000 ° C in a nitrogen atmosphere of 1 to 1.5 atmospheres. Keep it warm for 0.5 ⁇ 2h, continue to heat up to 2250 °C ⁇ 2400 °C, keep warm for 3.5 ⁇ 10 hours, cool down to 400 ⁇ 600 °C / h to 1900 °C ⁇ 2000 °C, keep warm for 0.5 ⁇ 2h, get the grown aluminum nitride Crystal
  • the grown aluminum nitride crystal was used as a seed crystal, and the substrate containing the seed crystal was placed on a second crucible.
  • the diameter of the hollow part of the temperature adjustment table was increased, and the temperature was raised to 400 to 600 ° C / h to 1900. °C ⁇ 2000 °C, keep warm for 0.5 ⁇ 2h, continue to heat up to 2250 °C ⁇ 2400 °C, keep warm for 3.5 ⁇ 10 hours, cool down to 400 ⁇ 600 °C / h to 1900 °C ⁇ 2000 °C, hold for 0.5 ⁇ 2h, get Aluminum nitride crystal.
  • the invention provides a device and a method for preparing aluminum nitride crystals.
  • the structure of the reaction chamber and the raw material cavity of the first crucible is used to reduce the nucleation, and the temperature of the center of the substrate is adjusted by using a temperature adjustment table, thereby forming an aluminum nitride unit
  • a substrate on which an aluminum nitride single crystal is formed is placed on a second crucible, and the characteristics of the reaction cavity and the structure cavity are used to increase the growth rate of the aluminum nitride single crystal to obtain an aluminum nitride crystal.
  • the aluminum nitride crystal does not contain impurities, has high quality, and is controllable in size, and can obtain a large-sized aluminum nitride crystal.
  • FIG. 1 and 2 are schematic structural diagrams of an apparatus for preparing an aluminum nitride crystal according to an embodiment of the present invention
  • FIG. 3 is a schematic structural diagram of a temperature adjustment platform according to an embodiment of the present invention.
  • FIG. 4 is a schematic structural diagram of a temperature adjustment platform according to an embodiment of the present invention.
  • FIG. 5 is a schematic structural diagram of a temperature adjustment platform according to an embodiment of the present invention.
  • FIG. 6 is a schematic diagram of an aluminum nitride crystal prepared according to an embodiment of the present invention.
  • FIGS. 1 to 2 are schematic structural diagrams of an apparatus for preparing aluminum nitride crystals according to an embodiment of the present invention.
  • the apparatus for preparing aluminum nitride crystals includes a first crucible 101 and a second crucible. 102, the substrate 103, and the temperature adjustment table 104;
  • the first crucible 101 includes a raw material cavity and a reaction cavity.
  • the diameter of the reaction cavity is larger than the diameter of the raw material cavity.
  • the raw material cavity is located at the bottom of the first crucible 101 and the reaction cavity is located at the opening of the first crucible 102.
  • the height of the raw material cavity of the first crucible 101 is 30 to 60 mm and the diameter is 15 to 45 mm.
  • the height of the reaction cavity of the first crucible 101 is 50 to 20 mm and the diameter is 30 to 50 mm.
  • the diameter of the reaction cavity is larger than that of the raw material cavity.
  • the diameter is 5 to 15 mm, and the wall thickness of the first crucible 101 is 2 to 5 mm.
  • the raw material cavity is used to store materials, namely aluminum nitride, which is a low temperature region, which can reduce the sublimation speed of aluminum nitride, the diameter of the reaction cavity is large, and the mass transmission area of the gas can be increased.
  • the larger volume of the cavity can reduce the partial pressure of aluminum vapor during nucleation, control the supersaturation at a lower level, and increase the overall temperature of the substrate 103 while increasing the temperature in this region, so that the temperature of the substrate 103 Above the temperature of the raw material cavity, the nucleation is reduced.
  • the substrate 103 covers the opening of the first crucible 101, so that the aluminum nitride crystal is condensed on the substrate 103 after the reaction chamber is sublimed;
  • the temperature adjusting table 104 has a hollow structure, and the side with the smallest diameter of the hollow portion is placed on the substrate 103 to adjust the contact area between the substrate 103 and the outside air.
  • FIG. 3 shows a schematic structural diagram of a temperature adjustment table in this embodiment.
  • the temperature adjustment table 104 is composed of a plurality of hollow cylinders. Layers increase. Among them, the diameter of the cylinder with the smallest diameter in the temperature adjustment table is 1 mm, and the diameter of the cylinder with the largest diameter is 25 mm.
  • FIG. 4 shows a schematic structural diagram of a temperature adjustment table in this embodiment.
  • the temperature adjustment table 104 is a multi-layer hollow cylinder, and the hollow portion is a cone structure.
  • the diameter of the top of the cone in the middle of the temperature control platform is 1 mm, and the diameter of the bottom of the cone is 25 mm.
  • FIG. 5 shows a schematic structural diagram of a temperature adjustment table in this embodiment.
  • the temperature adjustment table 104 is a plurality of plates with central openings, and each plate is opened in the middle. The diameter of the holes gradually increases. The diameter of the plurality of centrally-opened plates in the temperature adjustment table 104 ranges from 1 to 25 mm.
  • the maximum diameter of the temperature adjustment table 104 is between the diameter of the reaction chamber of the first crucible 101 and the diameter of the raw material chamber.
  • the effect of the temperature adjustment table 104 is the same.
  • the radial temperature field distribution of the substrate 103 can be adjusted so that the temperature of the substrate 103 increases linearly from the geometric center to the edge.
  • the center position of the substrate 103 is a very low temperature region. Since the gas flows from high temperature to low temperature, the gas flows to the center position of the substrate 103, and the aluminum vapor partial pressure in the center of the substrate 103 increases; at the same time, the crystals are at a lower temperature. Nucleation, so the crystal nucleates at the geometric center of the substrate 103, greatly reducing the nucleation rate, so that only one aluminum nitride single crystal is grown.
  • the second crucible 104 includes a raw material cavity and a reaction cavity, wherein the raw material cavity of the second crucible 104 is located at the bottom of the second crucible 104, and the diameter of the raw material cavity of the second crucible 102 is smaller than the diameter of the reaction cavity of the second crucible 102.
  • the height of the raw material cavity of the second crucible 102 is 30 to 60 mm and the diameter is 35 to 75 mm.
  • the height of the reaction cavity of the second crucible 102 is 50 to 20 mm and the diameter is 30 to 50 mm.
  • the wall thickness of the second crucible 102 I 2 ⁇ 5mm, the diameter of the raw material cavity in the second crucible 102 is 5 ⁇ 25mm larger than the diameter of the reaction cavity.
  • the single crystal prepared in the first crucible 101 is transferred to the second crucible together with the substrate.
  • the volume of the raw material cavity makes the material contained in the raw material cavity nitride.
  • the device for preparing aluminum nitride crystals further includes: crucible lid 105, crucible lid 105 It is placed at the opening of the second crucible 104.
  • the thickness of the crucible cover 105 is 1 to 3 mm.
  • the diameter of the crucible cover 105 is greater than or equal to the diameter of the second crucible 104. In this way, it is possible to prevent steam from diffusing to the outside of the crucible, reduce the partial pressure of gas, and cause waste of raw materials.
  • the device for preparing an aluminum nitride crystal uses the structure of the reaction chamber and the raw material cavity of the first crucible to reduce nucleation, and uses a temperature adjustment table to adjust the temperature of the center of the substrate to form an aluminum nitride single crystal. And the substrate forming the aluminum nitride single crystal is placed on the second crucible, and the characteristics of the reaction cavity and the structure cavity are used to increase the growth rate of the aluminum nitride single crystal to obtain the aluminum nitride crystal.
  • the aluminum nitride crystal does not contain impurities, has high quality, and is controllable in size, and can obtain a large-sized aluminum nitride crystal.
  • the invention provides a method for preparing an aluminum nitride crystal.
  • the method is applied to the above device for preparing an aluminum nitride crystal.
  • the method includes:
  • Step 1 Place aluminum nitride in the reaction chamber of the first crucible, place the substrate on the top of the first crucible, and place the side with the smallest diameter of the hollow part of the temperature adjustment table on the substrate. And the center of the temperature adjustment table coincides with the center of the substrate, and the temperature is raised to 2000 ° C to 3000 ° C in a nitrogen atmosphere of 1 to 1.5 atmospheres at a heating rate of 400 to 600 ° C / h, and the temperature is maintained for 3.5 to 10 hours. A single crystal of aluminum nitride is obtained at the center of the substrate;
  • step one an aluminum nitride single crystal having the same diameter as the hollow portion of the temperature control table can be obtained, and the diameter of the aluminum nitride single crystal can be 1 to 10 mm, as shown in FIG. 6.
  • the holding temperature is from 2250 ° C to 2400 ° C.
  • Step 2 Use the aluminum nitride single crystal as the seed crystal, increase the diameter of the hollow part of the temperature adjustment table, and heat up to 1900 ° C to 2000 ° C at a temperature increase rate of 400 to 600 ° C / h under a nitrogen atmosphere of 1 to 1.5 atmospheres. At °C, hold for 0.5 ⁇ 2h, keep warming to 2000 °C ⁇ 3000 °C, keep warm for 3.5 ⁇ 10 hours, reduce the temperature to 400 ⁇ 600 °C / h to 1900 °C ⁇ 2000 °C, and keep it for 0.5 ⁇ 2h.
  • Aluminum nitride crystal Aluminum nitride crystal
  • the second step can be repeated multiple times, and the diameter of the hollow part of the temperature control table is increased by 2 to 6 mm each time.
  • the aluminum nitride crystal can be sublimated, and the seed crystal will not be severely decomposed. It is ensured that there is a suitable supersaturation at the early stage of the high-temperature growth stage, and the aluminum nitride seed crystal is prevented from decomposing.
  • the number of cracks in the aluminum nitride crystal can be reduced by annealing at a lower temperature.
  • the holding temperature is from 2250 ° C to 2400 ° C.
  • Step 3 Use the grown aluminum nitride crystal as the seed crystal, and place the substrate containing the seed crystal on the second crucible, increase the diameter of the hollow part of the temperature adjustment table, and increase the temperature at a temperature of 400 ⁇ 600 ° C / h When warming to 1900 °C ⁇ 2000 °C, keep warm for 0.5 ⁇ 2h, continue to warm to 2250 °C ⁇ 2400 °C, keep warm for 3.5 ⁇ 10 hours, reduce temperature to 400 ⁇ 600 °C / h to 1900 °C ⁇ 2000 °C, keep warm for 0.5 ⁇ 2h, aluminum nitride crystals were obtained.
  • the large volume of the raw material cavity in the second crucible causes more aluminum nitride to be contained in the raw material cavity, which can ensure that the raw material has a sufficiently high sublimation rate, the volume of the reaction cavity is small, and the aluminum vapor partial pressure can be increased.
  • a larger supersaturation environment is formed to ensure a larger growth rate, so that the reaction proceeds in reverse, and a larger size aluminum nitride crystal is obtained.
  • the method further includes:
  • the aluminum nitride powder was heated to 1500 ° C. to 2000 ° C. for 3 to 6 hours under a nitrogen atmosphere, and repeated 2 to 5 times to obtain sintered aluminum nitride.
  • the structure of the reaction chamber and the raw material cavity of the first crucible is used to reduce nucleation, and the temperature of the center of the substrate is adjusted by using a temperature adjustment table to form an aluminum nitride single crystal.
  • the substrate forming the aluminum nitride single crystal is placed on the second crucible, and the characteristics of the reaction cavity and the structure cavity are used to increase the growth rate of the aluminum nitride single crystal to obtain the aluminum nitride crystal.
  • the aluminum nitride crystal does not contain impurities, has high quality, and is controllable in size, and can obtain a large-sized aluminum nitride crystal.

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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)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

La présente invention concerne un appareil et un procédé de préparation d'un cristal de nitrure d'aluminium, concernant le domaine technique de la préparation de matériau. L'appareil comprend : un premier creuset (101), un second creuset (102), un substrat (103), et une plateforme de régulation de température (104). Le premier creuset (101) comprend une chambre de matière première et une chambre réactionnelle ; le diamètre de la chambre réactionnelle est supérieur à celui de la chambre de matière première ; la chambre de matière première est située au fond du premier creuset (101) ; la chambre réactionnelle est située à l'ouverture du premier creuset (101). Le substrat (103) recouvre l'ouverture du premier creuset (101) de sorte qu'un cristal de nitrure d'aluminium peut se condenser sur le substrat (103) après sublimation dans la chambre réactionnelle. La plateforme de régulation de température (104) est une structure creuse, et le côté de la partie creuse ayant le diamètre minimal est placé sur le substrat (103), afin de régler la zone de contact entre le substrat (103) et l'air extérieur. Le second creuset (102) comprend une chambre de matière première et une chambre réactionnelle ; la chambre de matière première du second creuset (102) est située au fond du second creuset (102) ; le diamètre de la chambre de matière première du second creuset (102) est inférieur à celui de la chambre réactionnelle du second creuset (102).
PCT/CN2018/088423 2018-05-25 2018-05-25 Appareil et procédé de préparation d'un cristal de nitrure d'aluminium Ceased WO2019222997A1 (fr)

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PCT/CN2018/088423 WO2019222997A1 (fr) 2018-05-25 2018-05-25 Appareil et procédé de préparation d'un cristal de nitrure d'aluminium

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PCT/CN2018/088423 WO2019222997A1 (fr) 2018-05-25 2018-05-25 Appareil et procédé de préparation d'un cristal de nitrure d'aluminium

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111748844A (zh) * 2020-07-10 2020-10-09 中电化合物半导体有限公司 一种碳化硅单晶生长装置及碳化硅单晶的生长方法

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CN105951177A (zh) * 2010-06-30 2016-09-21 晶体公司 使用热梯度控制的大块氮化铝单晶的生长
JP2016020286A (ja) * 2014-07-14 2016-02-04 株式会社フジクラ ＡｌＮ単結晶の製造方法及びＡｌＮ単結晶を成長させるための基材
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CN111748844A (zh) * 2020-07-10 2020-10-09 中电化合物半导体有限公司 一种碳化硅单晶生长装置及碳化硅单晶的生长方法

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