CN105803515A - New process for gallium arsenide single crystal growth by VGF - Google Patents
New process for gallium arsenide single crystal growth by VGF Download PDFInfo
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Abstract
The invention provides a new process for gallium arsenide single crystal growth by VGF. The method comprises the following steps: gallium arsenide polycrystalline and seed crystal are placed in a PBN crucible, the crucible is placed in a quartz tube, and vacuum-pumping and sealing are carried out; heating is carried out for 1.5 hours, a first zone is heated to 1220 DEG C, a second zone is heated to 1230 DEG C, a third zone is heated to 1233 DEG C, a fourth zone is heated to 1235 DEG C, a fifth zone is heated to 1225 DEG C, a sixth zone is heated to 1222 DEG C, and insulation is carried out for 1 hour; the third zone is heated to 1253 DEG C, and insulation is carried out for 2 hours; the third zone is heated to 1262 DEG C, the fourth zone is heated to 1244 DEG C, the fifth zone is heated to 1225 DEG C, and insulation is carried out for 1.5 hours; and shoulder expansion, equal-diameter growth and ending are carried out. The new process for gallium arsenide single crystal growth by VGF can substantially shorten time for heating, melting materials and collecting seed crystal, so that production efficiency of the whole process is improved.
Description
Technical field
The present invention relates to single crystal preparation technical field, particularly a kind of VGF arsenide gallium monocrystal growth new technology.
Background technology
It is a kind of new method occurred in recent years that VGF (VGF) grows high-quality gallium arsenide, it is mainly characterized by being placed on by gallium arsenide polycrystal in PBN crucible, it is placed on sealed after being vacuumized in quartz ampoule again, then places into growth monocrystalline in single crystal growing furnace.The method compares with liquid encapsulate Czochralski technique (LEC) and horizontal Bridgman method (HB), there is equipment manufacturing cost low, easily realize programme-control, monocrystal rod need not be round as a ball, utilization rate is high, the monocrystalline of growth has the advantage such as relatively low dislocation density and higher integrity, uniformity, as the material of photoelectric material and High Speed ICs, is particularly subjected to the favor of device manufacturer.The usual step of the method is: the temperature of 6 thermals treatment zone of single crystal growing furnace was warmed up to each district near 1230 degree with tens hours, adjust after 4th district and 3 district's temperature are raised 2-3 degree by temperature and melted crystal with tens hours, then the 2-3 degree that 3rd district and 4th district rise is dropped back to, raise 2 district's temperature 2-3 degree and connect seed crystal with tens hours, take around the time in a couple of days, be finally shouldering and isodiametric growth.
Summary of the invention
It is an object of the invention to provide a kind of VGF arsenide gallium monocrystal growth new technology, it substantially reduces temperature increasing for melting materials and connects the time of seed crystal, thus improve production efficiency.
For achieving the above object, the present invention takes techniques below scheme:
A kind of VGF arsenide gallium monocrystal growth new technology, utilizes a single crystal growing furnace, and the heating region in this single crystal growing furnace is followed successively by the firstth district, the secondth district, the 3rd district, the 4th district, the 5th district and the 6th district from top to bottom；This technique comprises the following steps:
(1) shove charge and thermocouple:
Gallium arsenide polycrystal, seed crystal are loaded in PBN crucible, puts into quartz ampoule sealed after being vacuumized, make gallium arsenide polycrystal in this crucible to should the 3rd district；Set temperature-measuring heat couple respectively in this firstth district, the secondth district, the 3rd district, the 4th district, the 5th district and the 6th district, additionally also set temperature-measuring heat couple respectively at the head of this seed crystal and afterbody, shouldering portion distal end and crystal growth afterbody；
(2) heat up:
1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1233 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district is heated to, then insulation 1 hour with 1.5 hours；
(3) material:
Heat to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1253 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 2 hours；
(4) seed crystal is connect:
Heat to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1262 DEG C of the 3rd district, 1244 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 1.5 hours；
(5) shouldering:
Cool to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1255 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 3.5 hours；
Cool to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1250 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 15 hours；
Cool to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1233 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then with insulation 30 hours；
Control temperature to 1215 DEG C of the firstth district, 1225 DEG C of the secondth district, 1228 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1227 DEG C of the 5th district, 1224 DEG C of the 6th district, then insulation 35 hours；
(6) isodiametric growth ending:
Isodiametric growth ending is carried out by existing usual method.
Further, described crucible top is additionally provided with the secondary crucible of built-in gallium arsenide polycrystal, and this pair crucible bottom connects with described crucible；Corresponding described 4th district of this pair crucible；And further comprise the steps of: between described step (3) and step (4)
(31) top material is changed:
Control temperature to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1245 DEG C of the 3rd district, 1250 DEG C of the 4th district, 1245 DEG C of the 5th district, 1245 DEG C of the 6th district, then insulation 2 hours.
The invention has the beneficial effects as follows: VGF arsenide gallium monocrystal of the present invention growth new technology can be greatly shortened temperature increasing for melting materials and connect the time of seed crystal, thus improving the production efficiency of whole technique.
Accompanying drawing explanation
Fig. 1 is the structural representation of the heating region of the single crystal growing furnace of first embodiment of the invention.
Fig. 2 is the structural representation of the heating region of the single crystal growing furnace of second embodiment of the invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described further, but and is not used to restriction the scope of the present invention.
The present invention provides a kind of VGF arsenide gallium monocrystal growth new technology, utilize a single crystal growing furnace 10, as shown in Figure 1, this single crystal growing furnace 10 has heating region and controls the attemperating unit of this heating region temperature, and this heating region is followed successively by the first district the 4, the 5th district 5 and the 6th district 6 of district the 3, the 4th of the 1, second district the 2, the 3rd of district from top to bottom.VGF arsenide gallium monocrystal of the present invention growth new technology comprises the following steps:
(1) shove charge and thermocouple:
Gallium arsenide polycrystal, seed crystal are loaded in PBN crucible 7, puts into quartz ampoule 8 sealed after being vacuumized, make gallium arsenide polycrystal in this crucible 7 to should the 3rd district 3；Set temperature-measuring heat couple respectively in this district 5 of district the 4, the 5th of district the 3, the 4th of the 1, second district the 2, the 3rd of the firstth district and the 6th district 6, additionally also set temperature-measuring heat couple respectively at the head of this seed crystal and afterbody, shouldering portion distal end and crystal growth afterbody；
(2) heat up:
1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1233 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district is heated to, then insulation 1 hour with 1.5 hours；
(3) material:
Heat to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1253 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 2 hours；
(4) seed crystal is connect:
Heat to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1262 DEG C of the 3rd district, 1244 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 1.5 hours；
(5) shouldering:
Cool to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1255 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 3.5 hours；
Cool to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1250 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 15 hours；
Cool to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1233 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then with insulation 30 hours；
Control temperature to 1215 DEG C of the firstth district, 1225 DEG C of the secondth district, 1228 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1227 DEG C of the 5th district, 1224 DEG C of the 6th district, then insulation 35 hours；
(6) isodiametric growth ending:
Being undertaken by existing usual method, this pair crucible bottom connects with described crucible, and its technological parameter is prior art, therefore does not repeat them here.
It is more than concrete structure and the processing step of first embodiment of the invention, as shown in Figure 2, second embodiment of the invention VGF monocrystalline adopts two crucible methods, namely crucible 7 top is provided with the secondary crucible 9 of built-in gallium arsenide polycrystal, connect with described crucible 7 bottom this pair crucible 9, corresponding described 4th district 4 of this pair crucible 9.This is mainly for the GaAs material liquid volume principle less than solid volume, and to make crucible 7 monocrystalline of bottom be full of, reach expection length, secondary crucible 9 must be added and increase crystal weight, the material of lower crucible 7 is first changed during material, change the material of upper secondary crucible 9 again so that it is can flow in crucible 7 after internal polycrystal raw material fusing and be filled by crucible 7.Thus differing only in of second embodiment of the invention and first embodiment, further comprise the steps of: between described step (3) and step (4)
(31) top material is changed:
Control temperature to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1245 DEG C of the 3rd district, 1250 DEG C of the 4th district, 1245 DEG C of the 5th district, 1245 DEG C of the 6th district, then insulation 2 hours.
In sum, VGF arsenide gallium monocrystal of the present invention growth new technology first embodiment starts to connecing seed crystal complete from heating, adds up to 6 hours, second embodiment is also only with 8 hours, it was greatly shortened compared with 48 hours of prior art, while improve production efficiency, brings huge economic interests.
The above, be only presently preferred embodiments of the present invention, not the structure of the present invention is done any pro forma restriction.Every any simple modification, equivalent variations and modification above example made according to the technical spirit of the present invention, all still falls within the scope of technical scheme.
Claims (2)
1. a VGF arsenide gallium monocrystal growth new technology, utilizes a single crystal growing furnace, and the heating region in this single crystal growing furnace is followed successively by the firstth district, the secondth district, the 3rd district, the 4th district, the 5th district and the 6th district from top to bottom；It is characterized in that, comprise the following steps:
(1) shove charge and thermocouple:
Gallium arsenide polycrystal, seed crystal are loaded in PBN crucible, puts into quartz ampoule sealed after being vacuumized, make gallium arsenide polycrystal in this crucible to should the 3rd district；Set temperature-measuring heat couple respectively in this firstth district, the secondth district, the 3rd district, the 4th district, the 5th district and the 6th district, additionally also set temperature-measuring heat couple respectively at the head of this seed crystal and afterbody, shouldering portion distal end and crystal growth afterbody；
(2) heat up:
1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1233 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district is heated to, then insulation 1 hour with 1.5 hours；
(3) material:
Heat to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1253 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 2 hours；
(4) seed crystal is connect:
Heat to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1262 DEG C of the 3rd district, 1244 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 1.5 hours；
(5) shouldering:
Cool to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1255 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 3.5 hours；
Cool to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1250 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then insulation 15 hours；
Cool to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1233 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1225 DEG C of the 5th district, 1222 DEG C of the 6th district, then with insulation 30 hours；
Control temperature to 1215 DEG C of the firstth district, 1225 DEG C of the secondth district, 1228 DEG C of the 3rd district, 1235 DEG C of the 4th district, 1227 DEG C of the 5th district, 1224 DEG C of the 6th district, then insulation 35 hours；
(6) isodiametric growth ending.
2. VGF arsenide gallium monocrystal according to claim 1 growth new technology, it is characterised in that: described crucible top is additionally provided with the secondary crucible of built-in gallium arsenide polycrystal, and this pair crucible bottom connects with described crucible；Corresponding described 4th district of this pair crucible；And further comprise the steps of: between described step (3) and step (4)
(31) top material is changed:
Control temperature to 1220 DEG C of the firstth district, 1230 DEG C of the secondth district, 1245 DEG C of the 3rd district, 1250 DEG C of the 4th district, 1245 DEG C of the 5th district, 1245 DEG C of the 6th district, then insulation 2 hours.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107955971A (en) * | 2017-12-27 | 2018-04-24 | 有研光电新材料有限责任公司 | Shouldering method in Horizontal Bridgman Method arsenide gallium monocrystal pulling process |
| CN108103577A (en) * | 2017-12-28 | 2018-06-01 | 广东先导先进材料股份有限公司 | The synthetic method and synthesizer of a kind of gallium arsenide polycrystal |
| CN109252220A (en) * | 2018-12-04 | 2019-01-22 | 中国电子科技集团公司第四十六研究所 | A kind of VGF/VB arsenide gallium monocrystal furnace structure and growing method |
| WO2019109367A1 (en) * | 2017-12-08 | 2019-06-13 | 中国电子科技集团公司第十三研究所 | Device and method for rotational and continuous crystal growth by vgf process after horizontal injection and synthesis |
| CN111020689A (en) * | 2019-12-13 | 2020-04-17 | 广东先导先进材料股份有限公司 | Crystal growth apparatus and method |
| CN113957537A (en) * | 2021-10-20 | 2022-01-21 | 云南鑫耀半导体材料有限公司 | Growth device and method for rapidly growing low-dislocation gallium arsenide single crystal by combining VB method and VGF method |
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| CN1865527A (en) * | 2006-04-21 | 2006-11-22 | 罗建国 | Precise vertical temperature-difference gradient condensation single crystal growth device and method thereof |
| CN104073872A (en) * | 2014-06-26 | 2014-10-01 | 大庆佳昌晶能信息材料有限公司 | Process for growing high-quality compound semiconductor single crystal by means of rotation-vertical gradient freeze (R-VGF) method |
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| CN1865527A (en) * | 2006-04-21 | 2006-11-22 | 罗建国 | Precise vertical temperature-difference gradient condensation single crystal growth device and method thereof |
| CN104073872A (en) * | 2014-06-26 | 2014-10-01 | 大庆佳昌晶能信息材料有限公司 | Process for growing high-quality compound semiconductor single crystal by means of rotation-vertical gradient freeze (R-VGF) method |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019109367A1 (en) * | 2017-12-08 | 2019-06-13 | 中国电子科技集团公司第十三研究所 | Device and method for rotational and continuous crystal growth by vgf process after horizontal injection and synthesis |
| US10519563B2 (en) | 2017-12-08 | 2019-12-31 | The 13Th Research Institute Of China Electronics Technology Group Corporation | Device and method for continuous VGF crystal growth through rotation after horizontal injection synthesis |
| CN107955971A (en) * | 2017-12-27 | 2018-04-24 | 有研光电新材料有限责任公司 | Shouldering method in Horizontal Bridgman Method arsenide gallium monocrystal pulling process |
| CN108103577A (en) * | 2017-12-28 | 2018-06-01 | 广东先导先进材料股份有限公司 | The synthetic method and synthesizer of a kind of gallium arsenide polycrystal |
| CN109252220A (en) * | 2018-12-04 | 2019-01-22 | 中国电子科技集团公司第四十六研究所 | A kind of VGF/VB arsenide gallium monocrystal furnace structure and growing method |
| CN111020689A (en) * | 2019-12-13 | 2020-04-17 | 广东先导先进材料股份有限公司 | Crystal growth apparatus and method |
| CN113957537A (en) * | 2021-10-20 | 2022-01-21 | 云南鑫耀半导体材料有限公司 | Growth device and method for rapidly growing low-dislocation gallium arsenide single crystal by combining VB method and VGF method |
| CN113957537B (en) * | 2021-10-20 | 2024-04-30 | 云南鑫耀半导体材料有限公司 | Device and method for quickly growing low dislocation gallium arsenide monocrystal by combining VB method and VGF method |
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