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Patent US7750355 - Light emitting element structure using nitride bulk single crystal layer - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inAdvanced Patent SearchPatentsThe object of this invention is to provide a high-output type nitride light emitting device. The nitride light emitting device comprises an n-type nitride semiconductor layer or layers, a p-type nitride semiconductor layer or layers and an active layer therebetween, wherein a gallium-containing nitride...http://www.google.com/patents/US7750355?utm_source=gb-gplus-sharePatent US7750355 - Light emitting element structure using nitride bulk single crystal layerAdvanced Patent SearchPublication numberUS7750355 B2Publication typeGrantApplication numberUS 10/493,594PCT numberPCT/IB2002/004441Publication dateJul 6, 2010Filing dateOct 28, 2002Priority dateOct 26, 2001Fee statusPaidAlso published asCN1263206C, CN1300901C, CN1575533A, CN1575534A, EP1453158A1, EP1453158A4, EP1453159A1, EP1453159A4, US7057211, US7935550, US20040238810, US20040251471, US20080108162, WO2003036771A1, WO2003043150A1Publication number10493594, 493594, PCT/2002/4441, PCT/IB/2/004441, PCT/IB/2/04441, PCT/IB/2002/004441, PCT/IB/2002/04441, PCT/IB2/004441, PCT/IB2/04441, PCT/IB2002/004441, PCT/IB2002/04441, PCT/IB2002004441, PCT/IB200204441, PCT/IB2004441, PCT/IB204441, US 7750355 B2, US 7750355B2, US-B2-7750355, US7750355 B2, US7750355B2InventorsRobert Dwilinski, Roman Doradzinski, Jerzy Garczynski, Leszek Sierzputowski, Yasuo KanbaraOriginal AssigneeAmmono Sp. Z O.O., Nichia CorporationExport CitationBiBTeX, EndNote, RefManPatent Citations (114), Non-Patent Citations (142), Referenced by (3), Classifications (43), Legal Events (3) External Links: USPTO, USPTO Assignment, EspacenetLight emitting element structure using nitride bulk single crystal layerUS 7750355 B2Abstract The object of this invention is to provide a high-output type nitride light emitting device.
wherein the intermediate layer or the protective layer is formed by a supercritical ammonia method at 600� C. or less and comprises an alkali metal element.
the intermediate layer or the protective layer is formed by a supercritical ammonia method at 600� C. or less and comprises an alkali metal element,
wherein the intermediate layer or the protective layer is formed by a supercritical ammonia method at 600� C. or less and comprises an alkali metal element,
the intermediate layer or the protective layer is formed by a supercritical ammonia method at 600� C. or less and comprises an alkali metal element, said light emitting device is a semiconductor laser device and formed on said A-plane of the bulk single crystal GaN substrate,
TECHNICAL FIELD This invention relates to a structure wherein a single crystal nitride layer prepared by a supercritical ammonia is used as a substrate or an intermediate layer of light emitting devices such as a laser structure etc.
BACKGROUND ART In the laser structure, crystal defect or dislocation of a waveguide causes electron-hole pairs to make non-radiative recombination therein. Ideally, considering the laser function, the dislocation density in the waveguide should be 104/cm2 or less. However, in the present situation, the dislocation density can not be reduced less than 106/cm2 by using a vapor phase epitaxial growth (MOCVD and HVPE) or by using a repeated ELOG (Epitaxial lateral overgrowth) because the waveguide is grown on a heterogeneous substrate, such as sapphire substrate or SiC substrate.
Moreover, in case that the active layer deposited on the heterogeneous substrate is formed by a quantum well layer containing In, the active layer is influenced by the crystal condition of the n-type nitride layer as a base, therefore it is necessary to form an undoped GaN layer or super lattice structure layer as the base. On the other hand, when the p-type nitride layer is deposited on the active layer containing In, a protective layer is preferably formed to avoid the active layer degradation by evaporation of In therefrom. When the protective layer for GaN or AlGaN layer is formed, the protective layer is formed at a temperature from 800� C. to 900� C. which is lower than that at formation of the active layer. Accordingly, a resultant nitride layer will be in the form of amorphous, which influences the crystal condition of the optical guide layer and p-type clad layer formed thereon.
DISCLOSURE OF INVENTION (Problems to be Solved by the Invention)
the bulk single crystal having a lower dislocation density can be obtained by AMMONO method at a very low temperature (600� C. or less), compared with the bulk single crystal prepared by a vapor phase growth of the nitride at 1000� C. or higher, and
A desired temperature not causing damage to the active layer comprising nitride semiconductor containing In should be lower than a temperature at which the active layer comprising nitride semiconductor containing In is formed. The active layer comprising nitride semiconductor containing In is grown usually at 900� C. and that temperature or less does not cause damage to the active layer due to degradation etc. Therefore, by applying AMMONO method, the nitride is grown at 600� C. or less, preferably 550� C. or less. Therefore, the active layer containing In which comprises single crystal GaN or AlGaN layer can be formed without degradation.
In the present invention, the crystallization of gallium-containing nitride is carried out at a temperature of 100 to 800� C., preferably 300 to 600� C., more preferably 400 to 550� C. Also, the crystallization of gallium-containing nitride is carried out under a pressure of 100 to 10,000 bar, preferably 1,000 to 5,500 bar, more preferably 1,500 to 3,000 bar.
The term �gallium-containing nitride� in the specification means a compound which includes at least gallium and nitrogen atom as a consistent element. It includes at least the binary compound GaN, ternary compounds such as AlGaN, InGaN or also quaternary compounds AlInGaN, where the range of the other elements to gallium can vary, in so far as the crystallization growth technique of ammonobasic is not hindered.
The term �gallium-containing nitride bulk single crystal� means a gallium-containing nitride single crystal substrate on which an optic and electronic device such as LED or LD can be prepared by an epitaxial growing process such as MOCVD, HVPE or the like.
The term �a precursor of gallium-containing nitride�means a substance which contains at least gallium, and if needed, an alkali metal, an element of the Group XIII, nitrogen and/or hydrogen, or a mixture thereof, and examples of such a precursor includes metallic Ga, an alloy or an intermetallic compound of Ga, and a hydride, amide, imide, amidoimide or azide of Ga, which can form a gallium compound soluble in a supercritical ammonia solvent as defined below.
The term �gallium-containing feedstock� means a gallium-containing nitride or a precursor thereof.
The term �supercritical ammonia solvent� means a supercritical solvent which contains at least ammonia, and ion or ions of at least one alkali metal for dissolving gallium-containing nitride.
The term �mineralizer� means a supplier for supplying one or more of alkali metal ions (Li, K, Na or Cs) for dissolving gallium-containing nitride in the supercritical ammonia solvent.
The phrase �the dissolution of the gallium-containing feedstock by AMMONO method� means a reversible or irreversible process in which the above feedstock takes the form of a gallium compound soluble in the supercritical solvent such as a gallium complex compound. The gallium complex compound means a complex compound in which a gallium as a coordination center is surrounded by ligands, e.g., NH3 or derivatives thereof such as NH2 − and NH2 −.
The term �supercritical ammonia solution� means a solution including a soluble gallium-containing compound formed by the dissolution of the gallium-containing feedstock in the supercritical ammonia solvent. Based on our experiment, we have found that there is an equilibrium relationship between the gallium-containing nitride solid and the supercritical solution under a sufficiently high temperature and pressure atmosphere. Accordingly, the solubility of the soluble gallium-containing nitride can be defined as an equilibrium concentration of the above soluble gallium-containing nitride in the presence of solid gallium-containing nitride. In such a process, it is possible to shift this equilibrium according to change in temperature and/or pressure.
The phrase �negative temperature coefficient of the solubility� shown in the gallium-containing nitride in the supercritical ammonia 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 the 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 gallium-containing nitride in the supercritical ammonia solvent, at least, has a negative temperature coefficient within a range of 300 to 550� C., and a positive pressure coefficient within a range of 1 to 5.5 Kbar, respectively.
The phrase �oversaturation of the supercritical ammonia solution of gallium-containing nitride� means that the concentration of the soluble gallium compounds in the above supercritical ammonia solution is higher than a concentration in an equilibrium state, i.e., the solubility of gallium-containing nitride. In case of the dissolution of gallium-containing nitride in a closed system, such oversaturation can be achieved, according to a negative temperature coefficient or a positive pressure coefficient of the solubility, by raising the temperature or reducing the pressure.
The chemical transport from the lower temperature dissolution zone to higher temperature dissolution zone crystallization zone is important for gallium-containing nitride in the supercritical ammonia solution. The phrase �the chemical transport� means a sequential process including the dissolution of gallium-containing feedstock, the transfer of the soluble gallium compound through the supercritical ammonia solution, and the crystallization of gallium-containing nitride from the oversaturated supercritical ammonia solution. In general, a chemical transport process is carried out by a certain driving force such as a temperature gradient, a pressure gradient, a concentration gradient, difference in chemical or physical properties between a dissolved feedstock and a crystallized product, or the like. Preferably, the chemical transport in the process of the present invention is achieved by carrying out the dissolution step and the crystallization step in separate zones, on condition that the temperature of the crystallization zone is maintained higher than that of the dissolution zone so that the gallium-containing nitride bulk single crystal can be obtained by the processes of this invention.
The term �seed� has been described above. According to the present invention, the seed provides a region or area on which the crystallization of gallium-containing nitride is allowed to take place, and the growth quality of the crystal depends on the quality of the seed. Thus, the seed with good qualities is selected.
The term �spontaneous crystallization� means an undesirable phenomenon in which the formation and the growth of the core of gallium-containing nitride from the oversaturated supercritical ammonia solution occur at any site inside the autoclave, and the spontaneous crystallization also includes disoriented growth of the crystal on the surface of the seed.
The term �selective crystallization on the seed� means a step of allowing the crystallization to take place on the face of the seed, accompanied by substantially no spontaneous growth. This selective crystallization on the seed is essential for the growth of a bulk single crystal, it is also one of the conditions to form the intermediate layer by applying AMMONO method.
The wafer is thus placed in the higher temperature zone, and the feedstock in the lower temperature zone in the reaction system inside the autoclave. Dissolution of the feedstock in the lower temperature zone leads to the oversaturation. In the reaction system, a convection flow is generated, due to which the dissolved feedstock is transported to the higher temperature zone. Due to a lower solubility at the higher temperature zone, the dissolved feedstock becomes recrystallized on the wafer which is a seed. Recrystallization approached in this way results in forming a bulk single crystal layer. Moreover, a characteristic feature of this method, as compared to the methods by which nitride semiconductor is formed from a vapor phase growth at a temperature over 900� C., is the fact that it allows growth of nitride semiconductor at a temperature preferably 600� C. or less, and more preferably 550� C. or less. Due to this, in the wafer placed in the higher temperature zone a thermal degradation of the active layer containing In does not take place.
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a schematic sectional view of the end face of the nitride semiconductor laser device according to the present invention.
BEST MODE FOR CARRYING OUT THE INVENTION Further herein a detailed description of the embodiments of the present invention is provided.
In case that the protective layer 41 is formed, the single crystal AlGaN layer can be formed at a low temperature, i.e. from 500� C. to 600� C., by applying AMMONO method. P-type nitride layer can be formed without degradation of the active layer containing In.
EXAMPLE 1 First, a GaN substrate 1 of 2 inch diameter on C-plane as a growth face is placed in a MOCVD reactor. Temperature is set at 1050� C. Hydrogen is used as a carrier gas, and ammonia and TMG (thrimethylgallium) are used as gaseous materials.
(1) 4 μm thickness n-type GaN contact layer, doped with Si at the level of 3�1018/cm3.
(2) n-type clad layer, in the form of the superlattice of the total thickness being 1.2 μm, formed by alternate deposition of 25 angstroms thickness undoped Al0.1Ga0.9N layers and n-type GaN layers doped with Si at the level of 1�1019/cm3.
(5) a wafer is introduced into the reactor (autoclave) inside which is filled with a supercritical ammonia. Having been filled with the feedstock in the form of GaN of 0.5 g, ammonia of 14.7 g and mineralizer in the form of Li of 0.036 g, the autoclave (36 cm3) is tightly closed at a temperature 500� C. or less inside the autoclave. The internal autoclave is divided into two zones: the higher temperature zone and the lower temperature zone. In the higher temperature zone of 550� C. there is a wafer, whereas in the lower temperature zone of 450� C. there are feedstock in the form of GaN and Ga metal. The sealed autoclave is left for three days. Under the low temperature condition, in the supercritical ammonia 100 angstrom thickness single crystal GaN protective film is grown on the GaN barrier layer of the n-type active layer.
Then the wafer is taken out from the autoclave and set in the MOCVD reactor device at a temperature of 1050� C.
(8) 150 angstroms thickness p-type contact layer of p-type GaN doped with Mg at the level of 1�1020/cm3.
After the above layers are deposited, the formed wafer is subject to annealing in the MOCVD reactor device under the nitrogen atmosphere, at a temperature of 700� C., which additionally reduces resistance of the p-type nitride semiconductor layer or layers.
Next the p-type electrode 80 in the form of Ni/Au is formed on the p-type contact layer so that an ohmic contact would appear, and the n-type electrode 90 in the form of Ti/Al on the n-type contact layer. Then, the wafer is subject to the thermal processing at a temperature of 600� C. Next, pad electrode in the form of Ni(1000Å)-Ti(1000Å)-Au(8000Å) are laid on the p-type and n-type electrode. After a reflecting film 100 in the form of Sio2 and TiO2 is formed, each nitride semiconductor laser device is cut out from the wafer by scribing.
Each nitride semiconductor laser device manufactured in this way is equipped with a heat sink and the laser oscillation is carried out. Due to an increase of a COD level, prolonged continuous oscillation time is expected�with threshold current density: 2.0 kA/cm2, power output: 100 mW, preferably 200 mW, and 405 nm oscillation wavelength.
EXAMPLE 2 A single crystal GaN end face film of 1 μm thickness is grown on the only one light emitting end face on the stripe part, whereas other stages of production of the nitride semiconductor laser device are carried out similarly as in Example 1.
Each laser device manufactured in this way is equipped with a heat sink and the laser oscillation is carried out. Prolonged laser lifetime in continuous oscillation mode is expected�with threshold current density: 2.0 kA/cm2, power output: 100 mW and 405 nm oscillation wavelength�similar as in Example 1.
EXAMPLE 3 A SiO2 protective film in the form of lattice pattern is deposited on the surface of the top p-type contact layer. Next, etching of RIE method is carried out so as to uncover an end face of a resonator and the surface of the n-type contact layer. Under the condition of the SiO2 mask of 0.5 μm thickness formed on the surface of the p-type contact layer, the wafer is introduced into the reactor (autoclave) inside which is filled with a supercritical ammonia. In other respects, production of the nitride semiconductor laser device is carried out similarly as in Example 1.
Each laser device manufactured in this way is equipped with a heat sink and laser oscillation is carried out. Prolonged laser lifetime in continuous oscillation mode is expected�with threshold current density: 2.0 kA/cm2, power output: 100 mW and 405 nm oscillation wavelength�similarly as in Example 1.
INDUSTRIAL APPLICABILITY As described above, a bulk single crystal substrate by the supercritical ammonia can be used to form nitride semiconductor light emitting devices according to the present invention so that an efficient laser device can be obtained to form a laser device on the substrate having less crystal dislocation causing non-radiative recombination.
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