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Timestamp: 2016-05-26 22:32:14
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Matched Legal Cases: ['application No. 02802023', 'application No. 02802023', 'Application No. 02821230', 'Application No. 200580040008', 'application No. 02775396', 'Application No. 2004', 'Application No. 2004', 'application No. 2003', 'Application No. 2003']

Patent US7589358 - Phosphor single crystal substrate and method for preparing the same, and ... - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsA light emitting device having a phosphor substrate, which comprises nitride containing at least one element selected from Group XIII (IUPAC 1989) having a general formula XN, wherein X is at least one element selected from B, Al, Ga and In, a general formula XN:Y, wherein X is at least one element selected...http://www.google.com/patents/US7589358?utm_source=gb-gplus-sharePatent US7589358 - Phosphor single crystal substrate and method for preparing the same, and nitride semiconductor component using the sameAdvanced Patent SearchPublication numberUS7589358 B2Publication typeGrantApplication numberUS 10/514,429PCT numberPCT/JP2002/013079Publication dateSep 15, 2009Filing dateDec 13, 2002Priority dateMay 17, 2002Fee statusPaidAlso published asUS20060054076, WO2003098708A1, WO2003098757A1Publication number10514429, 514429, PCT/2002/13079, PCT/JP/2/013079, PCT/JP/2/13079, PCT/JP/2002/013079, PCT/JP/2002/13079, PCT/JP2/013079, PCT/JP2/13079, PCT/JP2002/013079, PCT/JP2002/13079, PCT/JP2002013079, PCT/JP200213079, PCT/JP2013079, PCT/JP213079, US 7589358 B2, US 7589358B2, US-B2-7589358, US7589358 B2, US7589358B2InventorsRobert Dwilinski, Roman Doradzinski, Jerzy Garczynski, Leszek Sierzputowski, Yasuo KanbaraOriginal AssigneeAmmono Sp. Z O.O., Nichia CorporationExport CitationBiBTeX, EndNote, RefManPatent Citations (138), Non-Patent Citations (88), Referenced by (12), Classifications (30), Legal Events (3) External Links: USPTO, USPTO Assignment, EspacenetPhosphor single crystal substrate and method for preparing the same, and nitride semiconductor component using the same
US 7589358 B2Abstract
A crucible made of the nickel alloy of an inner diameter of 10 mm is charged with 1 g of metallic gallium and 0.1 g of metallic Zn, followed by introducing the crucible into a high-pressure autoclave of an inner diameter 14 mm and a height of 70 mm. The autoclave is charged then in a dry glove box with LiNH2, sealed and evacuated of gases with a special system, and 4.9 g of ammonia is dropped into the reaction chamber. After re-sealing, the autoclave is placed in a furnace and heated to 550� C., with the pressure in the autoclave reaching about 4000 bar. The autoclave is allowed to stay in these conditions for 1 week, then the temperature is lowered to the room temperature, and consequently the pressure in the autoclave is lowered to about 10 bar. After evacuation of ammonia the autoclave is placed inside a dry glove box and the crucible removed. The crucible contents are washed with water, to allow hydrolysis and washing off LiNH2 in the form of well water-soluble LiOH. The solid residues from the crucible are dried and resulted in a phosphor of GaN:Zn type in the form of a white powder. Photographs of the phosphor taken by a field emission scanning electron microscope (25000� magnitude) illustrate many crystallites of the shape of hexagonal prism, indicating a good crystalline quality of the phosphor.
When a metal or its compound including at least one element selected from B, Al, Ga or In reacts with NH3 in conditions above its critical point (132� C., 112 bar), the nitride reaction essentially takes place, but its rate is not satisfactory. However, when the reaction environment is supplemented with at least one element selected from Group I and Group II (IUPAC 1989) and/or compounds thereof, such as hydrides, imides, amides and nitrides, the nitriding reaction becomes much faster and efficient. The Group I element may preferably be Li, Na or K, while the Group II element may preferably be Mg or Ca. Nitrides of the Group I elements may preferably include Li3N, Na3N, K3N, their amides may include LiNH2, NaNH2 and KNH2, and imides—Li2NH etc. Nitrides of the Group II elements may preferably include Mg3N2, Ca3N2, their amides may include Mg(NH2)2, Ca(NH2)2, and imides—CaNH etc. Thanks to the native nitrogen defects the nitride phosphor obtained according to the invention can emit light even when it is not intentionally doped.
FIG. 1 shows a relation between pressure and GaN solubility in the supercritical ammonia containing potassium amide (at molar ratio of KNH2:NH3=0.07) at T=400� C. and T=500� C.
The phrase “negative temperature coefficient of solubility” means that the solubility is expressed by a monotonically decreasing function of the temperature, when all other parameters are kept constant. Similarly, the phrase “positive pressure coefficient of solubility” means that the solubility is expressed by a monotonically increasing function of the pressure, when all other parameters are kept constant. Based on our research, the solubility of nitride in the supercritical ammonia-containing solvent has a negative temperature coefficient within a range of 300 to 550� C., and a positive pressure coefficient within the range of 1 to 5.5 kbar, respectively. For example, as shown in FIG. 2, after dissolution of feedstock in an autoclave kept for 8 days at the temperature 400� C. (i.e. after dissolution step), crystallization of gallium nitride may be achieved by increasing the temperature inside the autoclave to 500� C. (crystallization step). On the other hand, as shown in FIG. 3, after dissolution of a feedstock at increased pressure in an autoclave kept for 2 days at the level of 3.5 kbar (i.e. after dissolution step), crystallization of gallium nitride is achieved by means of reducing the pressure to 2 kbar in the autoclave (crystallization step).
High-pressure autoclave 1 (FIGS. 4 and 5), having the inner diameter of 40 mm, length equal to 480 mm (D/L= 1/12) and volume of 585 cm3, is charged with 30 g of feedstock in the form of GaN in the crucible in the dissolution zone 13, and GaN seed of the diameter of 1 inchφ obtained by HVPE method is placed in the crystallization zone 14 of the same autoclave. Next the autoclave 1 is filled with 1.2 g of 6N purity metallic gallium and 1.2 g of metallic Zn, and then 7 g of 3N purity metallic lithium (or 23 g of metallic sodium) as a mineralizer, and further 238 g of ammonia (SN) and finally closed. The autoclave 1 is introduced into the furnace unit 4 and heated to 200� C. for three days.
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