CN104233459A - Growth device for preparing aluminum nitride crystal by adopting sublimation method - Google Patents
Growth device for preparing aluminum nitride crystal by adopting sublimation method Download PDFInfo
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- CN104233459A CN104233459A CN201310254352.5A CN201310254352A CN104233459A CN 104233459 A CN104233459 A CN 104233459A CN 201310254352 A CN201310254352 A CN 201310254352A CN 104233459 A CN104233459 A CN 104233459A
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Abstract
The invention belongs to the field of crystal preparation, and provides a growth device for preparing an aluminum nitride crystal by adopting a sublimation method to realize the growth technological conditions of large-size and high-quality aluminum nitride monocrystals. The specific content is as follows: (a) the growth device for preparing the aluminum nitride crystal by adopting the sublimation method comprises a main heater, a top heater, a side shielding layer and a bottom shielding layer, wherein all the shielding layers are full-metal thermal reflection screens and independent from each other, and internal sizes are distributed in a ladder manner; (b) the growth device has two sets of independent heaters, the temperature of a growth area can be conveniently and accurately controlled by adjusting the power of the two heaters to meet the temperature field conditions needed by the growth of the aluminum nitride crystal; and (c) the heaters and the shielding layers adopt unique structure design to meet the conditions that (i) the processing technique is simple and the manufacturing cost is relatively low; (ii) the service life is long and the maintenance cost is low; and (iii) impurities are not easily introduced to pollute the environment while the production can be met.
Description
Technical field
The invention belongs to crystal preparation field, particularly a kind of growing apparatus of sublimation method to prepare aluminum nitride crystal.
Background technology
Aluminum nitride crystal is one of Typical Representative of third generation semiconductor material (aluminium nitride, gan, silicon carbide, zinc oxide, diamond etc.), be again the direct band gap in these materials, one of energy gap the widest (6.2 electron-volts); It has possessed very excellent optical, electrical, sound, mechanical properties simultaneously, has shown extremely wide application prospect and great economic benefit difficult to the appraisal.Subliming method (or physical vapor transport) prepares the most frequently used method of aluminum nitride crystal at present, and its primary process decomposes distillation under aluminium nitride material high temperature, then forms AlN single crystal at cold zone recrystallize.The method is prepared in aluminum nitride crystal process, because growth temperature is more than 2000 DEG C, and the temperature distribution of growth district has larger impact to the growth velocity of crystal, form and crystalline quality, therefore, requiring that growing apparatus can meet at growth district can hot conditions, again can comparatively accurately control temperature field.
Nearly ten years, along with the development of the high temperature such as silicon carbide, sapphire crystalline material technology of preparing, Medium Frequency Induction Heating Furnace has the advantages such as heating is fast, energy consumption is little, becomes the major equipment of these materials of growth.But aluminum nitride crystal growth is very responsive to temperature field condition.The whether suitable quality directly determining aluminum nitride crystal growth quality of temperature field condition.And Medium Frequency Induction Heating Furnace is mainly by the relative position changed with coil that moves up and down of crucible, adjust the thermo parameters method of vitellarium, be difficult to accurately control temperature field distribution, especially the temperature head of gasification zone and crystallizing field.Therefore, in order to reach, the technique explored needed for proper growth condition is more, the cycle is longer.To sum up, the growing apparatus being suitable for sublimation method to prepare aluminum nitride crystal is researched and developed very important.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of growing apparatus of sublimation method to prepare aluminum nitride crystal is provided, meet the growth technique condition of large size, high quality AlN single crystal.
The technical scheme realizing above-mentioned purpose is a kind of growing apparatus of sublimation method to prepare aluminum nitride crystal, be made up of primary heater (4), heater top (3), side screen layer (5), top screen layer (2) and end screen layer (6), wherein, all screen layers are all-metal heat reflection screen, each screen layer is separate, and interior dimensions is all by stepped distribution.
In technique scheme, heater top (3) is the disk being formed closely " W " shape by circular tungsten plate cutting processing, its two ends respectively with the solid welding of 2 extraction electrodes (1).
In technique scheme, primary heater (4) is the at high temperature overall closed cylinder be encircled into again after being cut into " square wave " shape by rectangle tungsten plate.
In technique scheme, primary heater (4) is connected solid welding with 3 extraction electrodes (1) respectively by the trisection of cylinder the same side.
In technique scheme, side shielding screen (5) is followed successively by the tungsten cylinder of 3-9 layer and the molybdenum cylinder of 3-6 layer from inside to outside, form via solid welding behind tungsten bar perforation location between cylinder, the highly stepped distribution of cylinder, the distance between adjacent cartridges is 3-15 millimeter.
In technique scheme, top screen layer (2) is 6-15 layer tungsten plectane and outside by inside is that 3-6 layer molybdenum plectane forms via solid welding behind tungsten bar perforation location, the stepped increase of diameter of tungsten, molybdenum plectane, the distance between adjacent two plectanes is 3-15 millimeter.
In technique scheme, end screen layer (6) is followed successively by tungsten disc, tungsten support, 6-15 layer tungsten plectane and 3-6 layer molybdenum plectane from top to bottom, via solid welding behind tungsten bar location between each assembly, wherein, the stepped increase of diameter of tungsten, molybdenum plectane, the distance between adjacent two plectanes is 3-15 millimeter.
In technique scheme, all solid weldings are argon arc solid welding.
This invention has following advantage and disadvantage:
(1) this invention is used for sublimation method to prepare aluminum nitride crystal, comprises two cover well heaters, accurately can be controlled the temperature of growth district by the heating power of both adjustment, easy to operate, meets the temperature field condition needed for aluminum nitride crystal growth;
(2) no matter be well heater or screen layer, both are processed by the plate cutting of tungsten, and technique is comparatively simple, and can easily process, manufacturing cost is lower;
(3) shielding screen effectively can reduce the loss of heat by radiation and convection type, and meanwhile, rational structure design reduces the screen layer impact bad because deformation brings;
(4) 3 screen layers are mutually independent, once there be damage, only need the screen layer that maintain and replace damages, the maintenance cost of device is lower;
(5) well heater of tungsten board making, not easy fracture, and high-temperature embrittlement phenomenon is not obvious, durable in use;
(6) the existing good high thermal resistance of whole device, not easily introduces impurity again, does not pollute the environment simultaneously, harmless.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the embodiment of the present invention;
Fig. 2 is the schematic diagram of primary heater in the embodiment of the present invention.
Embodiment
The invention provides a kind of growing apparatus of sublimation method to prepare aluminum nitride crystal.Below for the embodiment of a growing apparatus made of the present invention, the present invention will be further described.
Embodiment
A kind of growing apparatus of sublimation method to prepare aluminum nitride crystal in this embodiment, as shown in Figure 1, be made up of primary heater (4), heater top (3), side screen layer (5), top screen layer (2) and end screen layer (6), wherein, all screen layers are all-metal heat reflection screen, each screen layer is separate, and inside is all by stepped distribution.Primary heater (4) as shown in Figure 2, is processed by the tungsten plate of rectangle.The course of processing comprises: first carried out being laser-cut into " square wave " shape by 2 millimeters of thick tungsten plates, wherein, and upper and lower unit measure-alike; Then by cutting after tungsten plate at high temperature entirety be encircled into cylindrical shape, ensure between each unit mutually isolated, such structure can make the effective radiating area of this well heater increase simultaneously, and can ensure that in burner hearth, temperature is comparatively even.3 extraction electrode (1) intervals connect on the heaters uniformly, wherein 3 pilot holes (7) are opened in each junction, 2 millimeters, aperture, then, tungsten bar is positioned through hole, and be welded and fixed by argon arc welding, extraction electrode (1) passes top screen layer, through position tape insulation porcelain piece.Heater top (3) by thickness be the circular tungsten plate of 2 millimeters through being laser-cut into nearly " W " shape, two ends are drawn 2 extraction electrodes (1) and are fixed through argon arc welding.The extraction electrode (1) of heater top (3) and primary heater (4) all through top screen layer, through position tape insulation porcelain piece.Side screen layer (5) is made up of 6 layers of tungsten cylinder and 6 layers of molybdenum cylinder, and wherein, cylinder is 0 by thickness respectively.The tungsten plate of 5 millimeters and molybdenum plate at high temperature entirety surround and form, the spacing of cylinder 5 millimeters, highly stepped distribution, via solid welding behind tungsten bar perforation location between cylinder.By 9 layer thicknesses, to be the tungsten plectane of 1 millimeter and 3 layer thicknesses be that the molybdenum plectane of 1 millimeter forms on top screen layer (2), and plectane forms via solid welding behind tungsten bar perforation location, and tungsten, the stepped increase of molybdenum plectane diameter, the distance between adjacent two plectanes is 5 millimeters.End screen layer (6) is followed successively by that thickness is the tungsten disc of 5 millimeters from top to bottom, 3 tungsten supports, 9 layer thicknesses are the tungsten plectane of 1 millimeter and 3 layer thicknesses are the molybdenum plectane of 1 millimeter, by solid welding behind tungsten bar location between them, wherein, tungsten, the stepped increase of molybdenum plectane diameter, the distance between adjacent two plectanes is 3-15 millimeter.Growing apparatus after assembling, pushes up screen layer, realizes between end screen layer with side screen layer being combined comparatively closely, can effectively reduce thermal radiation and convection loss.
Whole growing apparatus is using the three-phase alternating current of industrial 380 volts as power supply, after the conversion circuit unit of power supply, convert it into low voltage, the three-phase electricity of big current and two phase electricity, and be connected with the extraction electrode of heater top with primary heater respectively, well heater can form resistance heating, and needs the heating power adjusting these two well heaters and then the temperature field condition met needed for aluminum nitride crystal growth according to growth technique.
Claims (8)
1. the growing apparatus of a sublimation method to prepare aluminum nitride crystal, be made up of primary heater (4), heater top (3), side screen layer (5), top screen layer (2) and end screen layer (6), wherein, all screen layers are all-metal heat reflection screen, each screen layer is separate, and interior dimensions is all by stepped distribution.
2. growing apparatus according to claim 1, is characterized in that, heater top (3) is the disk being formed closely " W " shape by circular tungsten plate cutting processing, two ends respectively with the solid welding of 2 extraction electrodes (1).
3. growing apparatus according to claim 1, is characterized in that primary heater (4) is the at high temperature overall closed cylinder be encircled into again after being cut into " square wave " shape by rectangle tungsten plate.
4. the growing apparatus according to claim 1 and 3, is characterized in that primary heater (4) is connected solid welding with 3 extraction electrodes (1) respectively by the trisection of cylinder the same side.
5. growing apparatus according to claim 1, it is characterized in that, side shielding screen (5) is followed successively by the tungsten cylinder of 3-9 layer and the molybdenum cylinder of 3-6 layer from inside to outside, form via solid welding behind tungsten bar perforation location between cylinder, the highly stepped distribution of cylinder, the distance between adjacent cartridges is 3-15 millimeter.
6. growing apparatus according to claim 1, it is characterized in that, top screen layer (2) is 6-15 layer tungsten plectane and outside by inside is that 3-6 layer molybdenum plectane forms via solid welding behind tungsten bar perforation location, the stepped increase of diameter of tungsten, molybdenum plectane, the distance between adjacent two plectanes is 3-15 millimeter.
7. growing apparatus according to claim 1, it is characterized in that, end screen layer (6) is followed successively by tungsten disc, tungsten support, 6-15 layer tungsten plectane and 3-6 layer molybdenum plectane from top to bottom, via solid welding behind tungsten bar location between each assembly, wherein, the stepped increase of diameter of tungsten, molybdenum plectane, the distance between adjacent two plectanes is 3-15 millimeter.
8. growing apparatus according to claim 1, is characterized in that all solid weldings are argon arc solid welding.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106149057A (en) * | 2015-03-10 | 2016-11-23 | 深圳大学 | The controlled aluminum nitride crystal growth device in temperature field and technique |
CN111188091A (en) * | 2020-02-17 | 2020-05-22 | 山东大学 | Thermal field for resistance method aluminum nitride crystal growth furnace and assembling method thereof |
CN114752999A (en) * | 2022-03-30 | 2022-07-15 | 深圳大学 | Equipment and method for preparing crystal |
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CN102245813A (en) * | 2008-12-08 | 2011-11-16 | Ii-Vi有限公司 | Improved axial gradient transport (AGT) growth process and apparatus utilizing resistive heating |
CN102605426A (en) * | 2012-03-14 | 2012-07-25 | 苏州先端稀有金属有限公司 | Thermal field structure for generating temperature difference in ultra-high temperature state |
CN102995116A (en) * | 2012-12-24 | 2013-03-27 | 上海昀丰新能源科技有限公司 | Aluminum nitride crystal preparation furnace and thermal-insulation device thereof |
CN203295659U (en) * | 2013-06-10 | 2013-11-20 | 深圳大学 | Growing device for preparing aluminum nitride crystals through sublimation method |
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Patent Citations (4)
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CN102245813A (en) * | 2008-12-08 | 2011-11-16 | Ii-Vi有限公司 | Improved axial gradient transport (AGT) growth process and apparatus utilizing resistive heating |
CN102605426A (en) * | 2012-03-14 | 2012-07-25 | 苏州先端稀有金属有限公司 | Thermal field structure for generating temperature difference in ultra-high temperature state |
CN102995116A (en) * | 2012-12-24 | 2013-03-27 | 上海昀丰新能源科技有限公司 | Aluminum nitride crystal preparation furnace and thermal-insulation device thereof |
CN203295659U (en) * | 2013-06-10 | 2013-11-20 | 深圳大学 | Growing device for preparing aluminum nitride crystals through sublimation method |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106149057A (en) * | 2015-03-10 | 2016-11-23 | 深圳大学 | The controlled aluminum nitride crystal growth device in temperature field and technique |
CN111188091A (en) * | 2020-02-17 | 2020-05-22 | 山东大学 | Thermal field for resistance method aluminum nitride crystal growth furnace and assembling method thereof |
CN111188091B (en) * | 2020-02-17 | 2021-09-03 | 山东大学 | Thermal field for resistance method aluminum nitride crystal growth furnace and assembling method thereof |
CN114752999A (en) * | 2022-03-30 | 2022-07-15 | 深圳大学 | Equipment and method for preparing crystal |
CN114752999B (en) * | 2022-03-30 | 2023-08-11 | 深圳大学 | Equipment and method for preparing crystals |
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