CN115012027A - Preparation method of grain-size-controllable aluminum nitride raw material for growing aluminum nitride single crystal - Google Patents
Preparation method of grain-size-controllable aluminum nitride raw material for growing aluminum nitride single crystal Download PDFInfo
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- CN115012027A CN115012027A CN202210748578.XA CN202210748578A CN115012027A CN 115012027 A CN115012027 A CN 115012027A CN 202210748578 A CN202210748578 A CN 202210748578A CN 115012027 A CN115012027 A CN 115012027A
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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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
- C30B29/38—Nitrides
Abstract
The invention belongs to the technical field of preparation of aluminum nitride crystals, and particularly relates to a preparation method of a controllable-particle-size aluminum nitride raw material for growing aluminum nitride single crystals, which comprises the following steps: loading aluminum nitride powder layer by layer, wherein each layer is separated by a tungsten plate during loading, the tungsten plates are fixed through tungsten rings, and an assembly body is obtained after loading is completed; putting the assembly into a constant temperature furnace, heating to 1900-2300 ℃, and keeping the temperature for 1-50 h under the protection of nitrogen or argon atmosphere; slowly cooling to room temperature, and sintering the aluminum nitride powder into an aluminum nitride polycrystalline sheet; and putting the aluminum nitride polycrystalline tablets into a crusher to be crushed and screened according to needs, and selecting polycrystalline particles with proper sizes according to crystal growth needs. Compared with the prior art, the granularity of the aluminum nitride raw material with the controllable grain diameter prepared by the method can be controlled at any time according to needs, and the consistency of the raw material can be better ensured in the crystal growth process.
Description
Technical Field
The invention belongs to the technical field of aluminum nitride crystal preparation, and particularly relates to a preparation method of a controllable-particle-size aluminum nitride raw material for growing aluminum nitride single crystals.
Background
The aluminum nitride crystal (AlN) belongs to the third generation semiconductor wide-gap semiconductor material, and has the advantages of wide gap, high breakdown electric field, high heat conductivity, high electron saturation rate, high radiation resistance and the like. In view of the advantages, the AlN crystal material has wide application prospect.
At present, the most common method for growing aluminum nitride crystals is Physical Vapor Transport (PVT), in which an aluminum nitride raw material is placed in a high-temperature region to sublimate into a vapor substance, and the vapor substance is transported from the surface of the raw material to a seed crystal in a low-temperature region to crystallize and grow the aluminum nitride crystal under the driving of a temperature gradient by controlling the temperature gradient of a growth chamber. Therefore, the quality of the aluminum nitride raw material is the key to growing high quality aluminum nitride crystals. The aluminum nitride raw material purified by simple sintering has compact texture, and is not beneficial to the sublimation of aluminum nitride and the growth of crystals.
The aluminium nitride crystal raw materials reported at present are simply sintered or sintered after adding a certain intermediate substance to change the density, porosity and the like of the aluminium nitride crystal raw materials, but the aluminium nitride raw materials produced by the methods are all in a rod shape (as shown in figure 1) same as that of a sintering container, the sintering container is highly matched with an aluminium nitride growth crucible and the produced aluminium nitride raw materials for crystal growth, and the sintered raw materials cannot be broken and have low efficiency. And will introduce a certain amount of intermediate species that control porosity.
Therefore, the existing porous bar for growing the aluminum nitride raw material is limited by the shape of the sintering material, the sintering material container and the growth crucible must be matched, the single sintering material is less, the efficiency is low, and the raw material sintered once can only be used for growing crystals once. The porosity of the porous material rod is influenced by various factors, and after the polycrystalline material rod is placed in the growth crucible, a large gap exists between the polycrystalline material rod and the wall of the growth crucible, so that heat transfer in the material in the growth process is influenced, and the growth is influenced.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a grain-size-controllable aluminum nitride raw material for growing aluminum nitride single crystals.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a grain diameter controllable aluminum nitride raw material for growing aluminum nitride single crystals comprises the following steps: and loading the aluminum nitride powder layer by layer, wherein each layer is separated by a tungsten plate during loading, the loading height of each layer is between 5mm and 60mm, and the thickness of the tungsten plate is between 0.3mm and 50 mm.
Preferably, according to the invention, the filling height of each layer is between 5mm and 30 mm.
Preferably, according to the invention, the tungsten plate has a thickness of 1 to 5 mm. The shape and the diameter of the tungsten plate are matched with the diameter of the tungsten ring.
The height of the tungsten ring is 10mm-800mm, preferably 100mm-300mm, and the diameter of the tungsten ring is 10 mm-600 mm, preferably 60mm-160 mm.
The tungsten ring may be circular, but is not limited to circular.
The gap is 0-50mm, preferably 1-10 mm.
The specific charging layer number and the number of tungsten rings are determined according to the capacity of the constant temperature furnace. The assembly body of tungsten ring and material can be overlapped from top to bottom according to the specific situation of the constant temperature furnace, also can be put on the same plain film in sequence, also can be overlapped from top to bottom and put horizontally and go on at the same time.
The constant temperature furnace preferably has a tungsten-molybdenum structure, but is not limited to the tungsten-molybdenum structure, and the temperature range of the constant temperature furnace needs to be 1800-2400 ℃ for long-term use.
Loading the assembly similar to the assembly shown in the figure 2 into a constant temperature furnace, heating to 1900-2300 ℃, and keeping the temperature between 1H and 50H under the protection of nitrogen or argon atmosphere;
slowly cooled to room temperature and the aluminum nitride powder is sintered into an aluminum nitride polycrystalline sheet, preferably 5-30mm thick. Fig. 3 is a sintered aluminum nitride polycrystalline tablet.
The polycrystalline tablets are placed in a crusher for crushing as required. Because the polycrystalline tablets are more easily broken than polycrystalline rods and substantially free of introduced impurities. And screening by using a vibrating screen after crushing, and selecting polycrystalline particles with proper sizes according to crystal growth requirements.
Fig. 4 shows a large polycrystalline grain, fig. 5 a medium polycrystalline grain, and fig. 6 a small polycrystalline grain.
Advantageous effects
The invention discloses a preparation method of a grain-size-controllable aluminum nitride raw material for growing aluminum nitride single crystals, which has the following beneficial effects compared with the prior art:
the porous bar for the growth of the aluminum nitride raw material in the prior art is limited by the shape of a sintering material, a sintering material container and a growth crucible must be matched, the single sintering material is less, the efficiency is low, and the raw material sintered once can only be used for crystal growth once. The porosity of the porous material rod is influenced by various factors, and after the polycrystalline material rod is placed in the growth crucible, a large gap exists between the polycrystalline material rod and the wall of the growth crucible, so that heat transfer in the material in the growth process is influenced, and the growth is influenced. The invention crushes the cake-shaped aluminum nitride polycrystal material into the raw material with certain granularity through the steps of grinding tools, crushing and the like, thereby solving the problems of the adaptability of the crucible for growth and the porosity of the material.
Compared with the prior art, the granularity of the aluminum nitride raw material with the controllable grain diameter prepared by the method can be controlled at any time according to needs, and the consistency of the raw material can be better ensured in the crystal growth process.
Drawings
FIG. 1: a physical diagram of an aluminum nitride polycrystalline material rod produced in the prior art;
FIG. 2: a schematic view of the structure of the assembly in example 1;
FIG. 3: a photomicrograph of the sintered aluminum nitride polycrystalline web of example 1;
FIG. 4: a physical photograph of the large crystalline particles obtained in example 1;
FIG. 5: a physical photograph of the medium polycrystalline particles obtained in example 1;
FIG. 6: a photomicrograph of the small polycrystalline particles obtained in example 1;
in the figure, 1: a gap; 2: a tungsten plate; 3: a tungsten ring; 4: aluminum nitride powder.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Example 1
A preparation method of a grain diameter controllable aluminum nitride raw material for growing aluminum nitride single crystal comprises the following steps:
(1) loading 4 layers of aluminum nitride powder, wherein each layer is separated by a tungsten plate 2 during loading, the loading height of each layer is 5mm, the thickness of the tungsten plate is 1mm, the tungsten plate is fixed through a tungsten ring 3, the height of the tungsten ring is 100mm, the diameter of the tungsten ring is 60mm, a gap 1 is reserved between each layer of aluminum nitride powder and the upper layer of the tungsten plate, the gap of the gap is 1mm, an assembly body is obtained after loading, the assembly bodies are stacked up and down, and the structural schematic diagram of the assembly body is shown in FIG. 2;
(2) putting the assembly obtained in the step (1) into a constant temperature furnace, heating to 1900 ℃, and keeping the temperature for 50 hours under the protection of nitrogen or argon atmosphere;
(3) slowly cooling to room temperature, sintering the aluminum nitride powder into an aluminum nitride polycrystalline sheet, wherein the polycrystalline sheet is 5 thick, and the physical diagram of the sintered aluminum nitride polycrystalline sheet is shown in FIG. 3;
(4) and (4) putting the aluminum nitride polycrystalline tablets obtained in the step (3) into a crusher to crush the tablets as required, because the polycrystalline tablets are easier to crush than polycrystalline rods and substantially free from impurities. Screening by using a vibrating screen after crushing, and selecting the polycrystalline particles with proper sizes according to crystal growth requirements.
Fig. 4 is a photograph of a large crystal grain, fig. 5 is a photograph of a medium crystal grain, and fig. 6 is a photograph of a small crystal grain.
The constant temperature furnace is of a tungsten-molybdenum structure, and the temperature range of the constant temperature furnace is 1800-2400 ℃ for long-term use.
Example 2
A preparation method of a grain diameter controllable aluminum nitride raw material for growing aluminum nitride single crystals comprises the following steps:
(1) loading 4 layers of aluminum nitride powder, wherein each layer is separated by a tungsten plate 2 during loading, the loading height of each layer is 30mm, the thickness of the tungsten plate is 5mm, the tungsten plate is fixed through a tungsten ring 3, the height of the tungsten ring is 300mm, the diameter of the tungsten ring is 160mm, a gap 1 is reserved between each layer of aluminum nitride powder and the upper layer of the tungsten plate, the gap of the gap is 10mm, an assembly body is obtained after loading, the assembly bodies are stacked up and down, and the structural schematic diagram of the assembly body is shown in FIG. 2;
(2) putting the assembly obtained in the step (1) into a constant temperature furnace, heating to 2300 ℃, and keeping the temperature for 1h under the protection of nitrogen or argon atmosphere;
(3) slowly cooling to room temperature, and sintering the aluminum nitride powder into an aluminum nitride polycrystalline sheet with the thickness of 30 mm;
(4) and (4) putting the aluminum nitride polycrystalline tablets obtained in the step (3) into a crusher to crush the tablets as required, because the polycrystalline tablets are easier to crush than polycrystalline rods and substantially free from impurities. And screening by using a vibrating screen after crushing, and selecting polycrystalline particles with proper sizes according to crystal growth requirements.
Example 3
A preparation method of a grain diameter controllable aluminum nitride raw material for growing aluminum nitride single crystals comprises the following steps:
(1) loading 4 layers of aluminum nitride powder, wherein each layer is separated by a tungsten plate 2 during loading, the loading height of each layer is 20mm, the thickness of the tungsten plate is 3mm, the tungsten plate is fixed through a tungsten ring 3, the height of the tungsten ring is 200mm, the diameter of the tungsten ring is 100mm, a gap 1 is reserved between each layer of aluminum nitride powder and the upper layer of the tungsten plate, the gap of the gap is 5mm, an assembly body is obtained after loading, the assembly bodies are stacked up and down, and the structural schematic diagram of the assembly body is shown in FIG. 2;
(2) putting the assembly body obtained in the step (1) into a constant temperature furnace, heating to 2000 ℃, and keeping the temperature for 30 hours under the protection of nitrogen or argon atmosphere;
(3) slowly cooling to room temperature, and sintering the aluminum nitride powder into an aluminum nitride polycrystalline sheet with the thickness of 20 mm;
(4) and (4) putting the aluminum nitride polycrystalline tablets obtained in the step (3) into a crusher to crush the tablets as required, because the polycrystalline tablets are easier to crush than polycrystalline rods and substantially free from impurities. Screening by using a vibrating screen after crushing, and selecting the polycrystalline particles with proper sizes according to crystal growth requirements.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (9)
1. A preparation method of a grain diameter controllable aluminum nitride raw material for growing aluminum nitride single crystals is characterized by comprising the following steps:
(1) loading aluminum nitride powder layer by layer, wherein each layer is separated by a tungsten plate during loading, the tungsten plates are fixed through tungsten rings, and an assembly body is obtained after loading is completed for later use;
(2) putting the assembly obtained in the step (1) into a constant temperature furnace, heating to 1900-2300 ℃, and keeping the temperature for 1-50 h under the protection of nitrogen or argon atmosphere;
(3) slowly cooling to room temperature, and sintering the aluminum nitride powder into an aluminum nitride polycrystalline sheet;
(4) and (4) putting the aluminum nitride polycrystalline tablets obtained in the step (3) into a crusher to be crushed and screened according to needs, and selecting polycrystalline particles with proper sizes according to crystal growth needs.
2. The method of producing a controlled grain size aluminum nitride starting material for growing an aluminum nitride single crystal according to claim 1, wherein in the step (1), the loading height of each layer is between 5mm and 60mm, and the thickness of the tungsten plate is between 0.3mm and 50 mm.
3. The method for producing a controlled-particle-diameter aluminum nitride starting material for growing an aluminum nitride single crystal according to claim 1, wherein in the step (1), the height of the tungsten ring is 10mm to 800mm, the diameter of the tungsten ring is 10mm to 600mm, and the shape and diameter of the tungsten plate are matched with the diameter of the tungsten ring.
4. The method of producing a controlled-particle-diameter aluminum nitride starting material for growing an aluminum nitride single crystal according to claim 3, wherein the tungsten ring is annular.
5. The method for producing a controlled-particle-diameter aluminum nitride starting material for growing an aluminum nitride single crystal according to claim 1, wherein in the step (1), a gap is left between each layer of the aluminum nitride powder and the upper tungsten plate, and the gap is 0 to 50 mm.
6. The method of producing a controlled-particle-diameter aluminum nitride starting material for growing an aluminum nitride single crystal according to claim 1, wherein the number of the specified charging layers and the number of the tungsten plates and the tungsten rings are determined depending on the capacity of the constant temperature furnace.
7. The method of claim 6, wherein the assembly is placed on a single flat plate in a constant temperature furnace in sequence, or stacked up and down and placed horizontally.
8. The method for preparing a controlled-particle-size aluminum nitride raw material for growing aluminum nitride single crystals as claimed in claim 1, wherein the constant temperature furnace has a tungsten-molybdenum structure, and the temperature of the constant temperature furnace is in the range of 1800 ℃ to 2400 ℃ for long-term use.
9. The method of producing a controlled-particle-diameter aluminum nitride starting material for growing an aluminum nitride single crystal according to claim 1, wherein in the step (3), the polycrystalline web is 5 to 30mm thick.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2004289065A (en) * | 2003-03-25 | 2004-10-14 | Nikko Materials Co Ltd | Silicon sintered body and its manufacturing method |
| CN101687709A (en) * | 2007-07-13 | 2010-03-31 | 日矿金属株式会社 | sintered silicon wafer |
| CN101570889A (en) * | 2008-04-29 | 2009-11-04 | 深圳大学 | Heat-insulation device using sublimation method to prepare aluminum nitride crystal |
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