Source: http://www.google.com/patents/US6592663?dq=6,411,947
Timestamp: 2016-07-23 20:15:39
Document Index: 44611222

Matched Legal Cases: ['art 3', 'art 3', 'art 3', 'art 3', 'art 3', 'art 3']

Patent US6592663 - Production of a GaN bulk crystal substrate and a semiconductor device formed ... - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsA method of making a bulk crystal substrate of a GaN single crystal includes the steps of forming a molten flux of an alkali metal in a reaction vessel and causing a growth of a GaN single crystal from the molten flux, wherein the growth is continued while replenishing a compound containing N from a...http://www.google.com/patents/US6592663?utm_source=gb-gplus-sharePatent US6592663 - Production of a GaN bulk crystal substrate and a semiconductor device formed on a GaN bulk crystal substrateAdvanced Patent SearchPublication numberUS6592663 B1Publication typeGrantApplication numberUS 09/590,063Publication dateJul 15, 2003Filing dateJun 8, 2000Priority dateJun 9, 1999Fee statusPaidAlso published asUS7250640, US7508003, US8591647, US20040031437, US20070012239, US20090173274, US20140044970, US20150152568Publication number09590063, 590063, US 6592663 B1, US 6592663B1, US-B1-6592663, US6592663 B1, US6592663B1InventorsSeiji Sarayama, Masahiko Shimada, Hisanori Yamane, Hirokazu IwataOriginal AssigneeRicoh Company Ltd.Export CitationBiBTeX, EndNote, RefManPatent Citations (3), Non-Patent Citations (4), Referenced by (150), Classifications (32), Legal Events (5) External Links: USPTO, USPTO Assignment, EspacenetProduction of a GaN bulk crystal substrate and a semiconductor device formed on a GaN bulk crystal substrate
US 6592663 B1Abstract
What is claimed is: 1. A method of producing a single crystal body of a group III nitride, comprising:
forming a molten flux of a volatile metal element in a pressurized reaction vessel confining therein said molten flux together with an atmosphere containing N (nitrogen), such that said molten flux contains a group III element in addition to said volatile metal element; growing a nitride of said group III element in the form of a single crystal body in said molten flux; and supplying a compound containing N directly into the atmosphere in said reaction vessel from a source located outside said reaction vessel. 2. A method as claimed in claim 1, wherein said compound comprises N2 and NH3.
an forming a molten flux of K in a pressurized reaction vessel confining therein said molten flux together with an atmosphere containing N (nitrogen), such that said molten flux contains Ga in addition to K; and precipitating a single crystal body of cubic GaN in said molten flux. 18. A method as claimed in claim 17, further comprising the step of supplying a compound containing N (nitrogen) into said reaction vessel from an external source outside said reaction vessel.
19. A method as claimed in claim 17, wherein said precipitation is conducted by controlling a temperature of a melt surface of said molten flux at 650-850� C.
forming a molten flux of a volatile metal element in a pressurized reaction vessel confining therein said molten flux together with an atmosphere containing N (nitrogen), such that said molten flux contains a group III element in addition to said volatile metal element; growing a nitride bulk crystal of said group III element in said molten flux; and supplying a compound containing N directly into the atmosphere in said reaction vessel from a source located outside said reaction vessel. 21. A method as claimed in claim 20, wherein said compound comprises N2 and NH3.
forming a molten flux of K in a pressurized reaction vessel confining therein said molten flux together with an atmosphere containing N (nitrogen), such that said molten flux contains Ga in addition to K; and growing a bulk crystal of GaN of a cubic crystal system at a melt surface of said molten flux. 37. A method as claimed in claim 36, further comprising the step of supplying a compound containing N (nitrogen) into said reaction vessel from a source located outside said reaction vessel.
38. A method as claimed in claim 36, wherein said precipitation is conducted by controlling a temperature of said melt surface at 650-850� C.
a pressurized reaction vessel having a space therein for holding a crucible; a supply line connected to said reaction vessel, said supply line supplying a pressurized gas of a compound containing N (nitrogen) directly into an atmosphere in said reaction vessel; and a heater disposed outside said reaction vessel, said heater heating said reaction vessel externally so as to form a molten flux of a volatile metal element and a group III element in said crucible. 40. An apparatus as claimed in claim 39, further comprising a pressure-resistant vessel enclosing said reaction vessel.
After the formation of the SiO2 mask pattern 4, the upper GaN layer part 3 b is formed by an epitaxial lateral overgrowth (ELO) process in which the layer 3 b is grown laterally on the SiO2 mask 4. Thereby, desired epitaxy is achieved with regard to the lower GaN layer part 3 a at the opening 4A in the SiO2 mask pattern 4. By growing the GaN layer part 3 b as such, it is possible to prevent the defects, which are formed in the GaN layer part 3 a due to the large lattice misfit between GaN and sapphire, from penetrating into the upper GaN layer part 3 b. On the upper GaN layer 3 b, a strained super-lattice structure 5 having an n-type Al0.14Ga0.86N/GaN modulation doped structure is formed, with an intervening InGaN layer 5A of the n-type having a composition In0.1Ga0.9N interposed between the upper GaN layer part 3 b and the strained superlattice structure 5. By providing the strained superlattice structure 5 as such, dislocations that are originated at the surface of the sapphire substrate 1 and extending in the upward direction are intercepted and trapped.
On the upper cladding layer 8, another strained superlattice structure 9 of a p-type Al0.14Ga0.86N/GaN modulation doped structure is formed such that the superlattice structure 9 is covered by a p-type GaN cap layer 10. Further, a p-type electrode 11 is formed in contact with the cap layer 10 and an n-type electrode 12 is formed in contact with the n-type GaN buffer layer 3 b. It is reported that the laser diode of FIG. 1 oscillates successfully with a practical lifetime, indicating that the defect density in the active layer 7 is reduced successfully.
With regard to the art of growing a bulk crystal GaN, there is a successful attempt reported by Porowski (Porowski, S., J. Crystal Growth 189/190 (1998) pp.153-158, in which a GaN bulk crystal is synthesized from a Ga melt under an elevated temperature of 1400-1700� C. and an elevated N2 pressure of 12-20 kbar (1.2-2 GPa). This process, however, can only provide an extremely small crystal in the order of 1 cm in diameter at best. Further the process of Porowski requires a specially built pressure-resistant apparatus and a long time is needed for loading or unloading a source material, or increasing or decreasing the pressure and temperature. Thus, the process of this prior art would not be a realistic solution for mass-production of a GaN bulk crystal substrate. It should be noted that the reaction vessel of Porowski has to withstand the foregoing extremely high pressure, which is rarely encountered in industrial process, under the temperature exceeding 1400� C.
According to the process of Yamane, a metallic Ga source and a NaN3 (sodium azide) flux are confined in a pressure-resistance reaction vessel of stainless steel together with a N2 atmosphere, and the reaction vessel is heated to a temperature of 600-800� C. and held for a duration of 24-100 hours. As a result of the heating, the pressure inside the reaction vessel is elevated to the order of 100 kg/cm2 (about 10 MPa), which is substantially lower than the pressure used by Porowski. As a result of the reaction, GaN crystals are precipitated from the melt of a Na—Ga system. In view of the relatively low pressure and low temperature needed for the reaction, the process of Yamane et al. is much easier to implement.
Referring to FIG. 3, the growth apparatus 100 includes a pressure-resistant reaction vessel 101 typically of a stainless steel having an inner diameter of about 75 mm and a length of about 300 mm and accommodates therein a crucible 102 of Nb or BN. As will be explained later, the crucible 102 is loaded with a starting material of metallic Ga and a NaN3 flux and is confined in the reaction vessel 101 together with an N2 atmosphere 107. Further, the reaction vessel 101 is supplied with N2 or a gaseous compound of N from an external source via a regulator valve 109 and an inlet 108. The reaction vessel 101 thus loaded with the starting material in the crucible 102 is heated by energizing heaters 110 and 111 to a temperature of 650-850� C., and the pressure inside the reaction vessel is regulated to a moderate value of about 5 MPa by controlling the valve 109. By holding the temperature and the pressure, a precipitation of GaN bulk crystal takes place from a Na—Ga melt, which is formed in the crucible 102 as a result of the melting of the starting material.
With the growth of the GaN crystals, a particularly with the growth of the GaN single crystal 102B, N in the atmosphere is consumed and the pressure inside the reaction vessel gradually falls as a result of depletion of N in the atmosphere. Thus, in the present embodiment, the depletion of N in the atmosphere 107 is compensated for by replenishing N2 or a compound of N such as NH3 from an external source. Thereby, the growth of the GaN single crystal 102B continues at the melt free surface and a large GaN single crystal suitable for use in an optical semiconductor device such as a laser diode or light-emitting diode as a GaN bulk crystal substrate is obtained. The construction of FIG. 3 can easily produce the GaN single crystal 102B with a thickness of 100 μm or more. The GaN single crystal 102B thus formed at the temperature of 650-850� C. has a hexagonal crystal symmetry.
Due to the increased temperature at the bottom part of the crucible 102, undesirable precipitation of GaN crystals on bottom surface of the crucible 102 is minimized, and the growth of the GaN bulk crystal 102B on the melt surface is promoted substantially. When a GaN fine crystal 102C is formed, such a GaN fine crystal 102C is immediately dissolved into the melt 102A and no substantial deposition occurs on the bottom part of the crucible 102. Further, the intermetallic compound of GaNa, formed at a temperature lower than about 530� C., acts also as the source of Ga and Na in the melt 102A.
By providing the pressure vessel 112 outside the reaction vessel 101, the pressurized reaction vessel 101 is supported from outside and the design of the reaction vessel 101 becomes substantially easier. As represented in FIG. 10, there is provided a thermal insulator 115 between the heater 110 or 111 and the outer pressure vessel 112 and the temperature rise of the pressure vessel 112 is avoided. Thereby, the pressure vessel 112 maintains a large mechanical strength even when the inner, reaction vessel 101 is heated to the temperature exceeding 600 or 700� C. In order to avoid the decrease of mechanical strength, it is possible to provide a water cooling system (not shown) on the outer pressure vessel 112.
In any of the foregoing first through tenth embodiments, the grown of the GaN bulk crystal 102B has been achieved at the temperature of 650-850� C. under the presence of a Na flux. As mentioned before, the GaN bulk crystal 102B thus obtained has a symmetry of hexagonal crystal system.
On the other hand, the inventor of the present invention has discovered that a cubic GaN crystal is obtained as the bulk GaN-crystal 102B provided that the growth is made at a temperature of less than 600� C. under the presence of Na, or when the growth is made at a temperature of 650-850� C. under the presence of K. K may be introduced into the system in the form of a high-purity metallic K starting material, similarly to the case represented in FIG. 4A.
From the x-ray diffraction peak position data, it was confirmed that the cubic GaN bulk crystal 102B thus formed has a cubic lattice constant a0 of 4.5063�0.0009 Å. FIG. 19 shows x-ray diffraction intensity data obtained for a GaN bulk crystal grown by the apparatus of FIG. 3 as the bulk crystal 102B at a temperature of 750� C. under the total pressure of 7 MPa in the reaction vessel 101. In FIG. 19, it should be noted that the Of represents the structural factor obtained from the diffraction intensity data for each of the reflections (h k 1) and s represents the error factor of the measurement, while Fc represents the structural factor calculated from a cubic zinc blende structure. A reliability factor, R, of 2.1% demonstrates the well agreement of Of and Fc, where R is defined as:
In view of increasing defect density in the GaN crystals grown at low temperatures, and further in view of the fact that a mixture of cubic GaN and hexagonal GaN appears when the growth of the GaN bulk crystal is conducted at the temperature of 600� C. or lower under presence of Na flux, it is preferred to grow a cubic GaN bulk crystal at the temperature of 650-850� C. under presence of a K flux.
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