JP2005097022A - Synthetic method for group iiib nitride - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a synthetic method for nitride in a simple process using inexpensive starting raw materials for the purpose of solving the problems in the conventional synthesis method for group IIIB nitride particulates, and to provide group IIIB nitride particulates having light emitting properties. <P>SOLUTION: In the synthetic method for group IIIB nitride, a group IIIB element-containing compound and a nitrogen-containing compound are dissolved into a solvent, thereafter, the solvent is evaporated, the obtained uniform mixture is heated to reduce the group IIIB element-containing compound, and, the group IIIB elements are nitrided with nitrogen in the nitrogen-containing compound. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a method for synthesizing a group IIIB nitride using a wet preparation method of raw materials and a reduction nitriding method.

  GaN and BN, which are group IIIB nitrides, have attracted attention as ultraviolet emitters and are currently being actively studied. However, in most of these reports, IIIB nitrides are synthesized as thin films, and there are still few studies on powders and nanoparticles that exhibit physically unique properties. The conventional process for producing a thin film requires a very expensive apparatus, and further has a drawback that it is difficult to form a film on a complicated shape.

  It has been reported that hexagonal BN emits light blue when subjected to high temperature heat treatment in the presence of carbon and hydrogen (Non-patent Document 1). This method has a problem that a high temperature is required and the carbon content cannot be controlled.

As for GaN particles, the following synthesis methods have been reported so far.
(1) Method of reacting ammonia gas with Ga, GaCl ₃ , Ga ₂ O ₃ , gallium nitrate hydrate, gallium dialkyldithiocarbamate, gallium triisopropoxide, etc. (Non-patent Document 2, Patent Documents 1 to 6) . In this reaction, corrosive ammonia gas is used as a nitrogen source. Further, the obtained primary particles are all in the order of μm.
(2) Reaction method of Ga and NaN ₃ (Non-patent Document 3). The azide NaN ₃ used as a nitrogen source in this reaction reacts with acid to generate toxic and explosive hydroazide. In addition, it easily reacts with other metals and produces highly explosive salts, which are difficult to handle.
(3) A benzene-thermal reaction method between GaCl ₃ and Li ₃ N (Non-patent Document 4). Li ₃ N has low oxidation resistance and is difficult to handle. In addition, since the benzene-thermal method uses a pressure vessel, large-scale synthesis is impossible.
(4) A method of synthesizing nanoparticles by thermally decomposing tris (dimethylamino) gallium in trioctylamine (Patent Document 3). This compound is a special compound, and it is difficult to control the reaction, which causes a problem in industrial mass production.

K. Era, F. Minami, and T. Kuzuba, “Fast Luminescence from Carbon-Related Defects of Hexagonal Boron Nitride”, Journal of Luminescence, Vol. 24/25, pp71-74 (1981) K. Hara, Y. Matsuno and Y. Matsuo, “Vaper Phase Synthesis of Fluorecsent Gallium Nitride Powders”, Japanese Journal of Applied Physics Vol. 40, pp.L242-L244 (2001) Hisanori Yamane, Masato Aoki, Shoji Tairayama, "Growth of GaN single crystals by the flux method", Applied Physics, Vol. 71, pp.548-522, (2002) Y.Xie, Y. Qian, W. Wang, S. Zhan, “A Benzene-Thermal Synthetic Route to Nanocrystalline GaN,” Science, Vol.272, pp.1926-1927 JP 2000-198978 A JP 2001-151504 A JP 2002-029713 A JP 2002-029714 A JP 2003-34510 A JP 2003-63810 A Japanese Patent Laid-Open No. 2002-220213

  In general, when a phosphor is put into practical use as an optical / electronic device, the most suitable form is a particle. In particular, if the phosphor is a nanoparticle with a particle size of 10 nm or less, unlike the bulk, electrons and holes are confined in a very narrow space, so excitons (electron-hole pairs) are generated stably. A quantum confinement effect that increases the quantum efficiency of light emission is expected. Among group IIIB nitrides, GaN having a band gap in the ultraviolet region is expected to be widely used as a display phosphor such as a field emission display.

  However, in general, there are many defects such as dangling bonds on the surface of the nanoparticles, and the excitons are almost non-radiatively deactivated due to non-radiation deactivation. In addition, since there is a large proportion of atoms appearing on the surface, there is a tendency to agglomerate to reduce the surface energy, and it has been reported that imperfect chemical bonds generated by this aggregation reduce luminescence as well as defects. ing. In addition, when micron-sized particles are mechanically crushed into nano-size, dislocations enter the crystal and the emission intensity decreases.

  In the conventional method for synthesizing group IIIB nitride fine particles, ammonia having strong corrosivity is mainly used as a nitrogen source. Some studies using sodium azide have also been reported. Although sodium azide itself is not explosive, it reacts with acid to produce toxic and explosive hydroazide. Furthermore, it can be said to be a very dangerous chemical because it reacts easily with other metals to produce highly explosive salts. In addition, a special pressure vessel or vacuum chamber is required for the reaction apparatus.

  In order to solve the problems of the conventional method for synthesizing group IIIB nitride fine particles as described above, the present invention provides a method for synthesizing nitride by a simple process using an inexpensive starting material, and has a light emitting characteristic. It is an object to provide group IIIB nitride fine particles.

  The present inventors have prepared a group IIIB nitride by preparing a relatively safe starting material by a wet method without requiring a high temperature, and subjecting this to a reduction nitriding treatment using a nitrogen-containing compound such as urea. I found.

  By the method of the present invention, it is possible to produce group IIIB nitride fine particles such as hexagonal BN, disordered layer type BN, GaN, Ga-In-N, and composite fine particles including GaN nanoparticles in hexagonal BN fine particles. is there. The fine particles are usually particles having a particle diameter of 1 nm to 1 μm, and the ultrafine particles are particles having a particle diameter of 1 nm to 100 nm. In the present invention, the nanoparticle means a particle of about 1 nm to 50 nm. GaN included in the hexagonal BN particles is a nanoparticle of about 5 to 10 nm. In the present invention, the size of these particles is shown as the number average particle size of primary particles observed with a transmission electron microscope (TEM). Group IIIB refers to B, Al, Ga, and In elements belonging to Group IIIB of the periodic table.

  That is, the present invention comprises (1) dissolving a group IIIB element-containing compound and a nitrogen-containing compound in a solvent, and then heating the homogeneous mixture obtained by evaporating the solvent to reduce the group IIIB element-containing compound to reduce nitrogen A method for synthesizing a group IIIB nitride, characterized in that a group IIIB element is nitrided with nitrogen of a compound.

  The present invention also provides (2) a method for synthesizing a group IIIB nitride according to (1) above, wherein the group IIIB nitride is a hexagonal BN, GaN, or Ga—In—N solid solution.

Further, the present invention provides (3) III in (1) above, wherein the nitrogen-containing compound is urea.
This is a method for synthesizing a group B nitride.

  The present invention also provides (4) a method for synthesizing a group IIIB nitride according to any one of the above (1) to (3), wherein the solvent is water, alcohol, or a hydrocarbon compound, It is.

  The present invention is also (5) the method for synthesizing a group IIIB nitride according to (1) above, wherein the group IIIB nitride is fine particles.

  The present invention is also (6) the method for synthesizing group IIIB nitride according to (1) above, wherein the group IIIB nitride is nanoparticles having a number average particle diameter of 1 nm to 50 nm.

  The present invention is also (7) the method for synthesizing a group IIIB nitride according to (1) above, wherein the group IIIB nitride is micron-sized particles.

  Moreover, this invention controls the particle size of the produced | generated particle | grains by adjusting the molar ratio of (8) IIIB group element containing compound and a nitrogen-containing compound, Any of said (5)-(7) characterized by the above-mentioned. A method for synthesizing a group IIIB nitride as described above.

  The present invention is also (9) the method for synthesizing a group IIIB nitride according to (1) above, wherein the group IIIB nitride is boron nitride (BN) and is a sponge-like lump.

  Further, the present invention is the (III) Group IIIB nitride according to (1), wherein the Group IIIB nitride is a turbulent structure type boron nitride (BN) fine particle containing oxygen and exhibits fluorescence characteristics This is a synthesis method.

  The present invention also provides (11) a method for synthesizing a group IIIB nitride according to item (1), wherein the group IIIB nitride is GaN nanoparticles and exhibits fluorescence characteristics.

  The present invention is also characterized in that (12) the group IIIB nitride is a composite particle composed of a composite of GaN and hexagonal BN or a composite of Ga-In-N solid solution and hexagonal BN. (4) A method for synthesizing a group IIIB nitride.

  The present invention is also (13) a method for synthesizing a group IIIB nitride according to (4) above, wherein the composite particles include GaN nanoparticles monodispersed in hexagonal BN.

  According to the method of the present invention, unlike the conventional fine particle production method mainly produced by a gas phase reaction or a spray method, the raw material is once dissolved in a solvent and the solvent is evaporated to prepare a homogeneous mixture. Fine particles, particularly particles having a primary particle size of nanometer size can be directly obtained by reductive nitriding while the powder mixture is held in a heating furnace. This is because when the GaN or BN single-phase particles are synthesized by the method of the present invention, the GaN particles are synthesized in the matrix of the nitrogen-containing compound. It is presumed that since the distance from the generated GaN particles is too large to be bonded, the fine particle size is maintained even after the reaction is completed. Similarly, in the case of BN / GaN composite particles, GaN particles are generated in the base of the BN particles, so that the GaN particles cannot be brought close to each other by pushing out the BN particles. It is assumed that the GaN fine particles are taken into the BN particles as they are.

INDUSTRIAL APPLICABILITY The present invention can provide a group IIIB nitride phosphor used as an optical / electronic device by a safe and inexpensive method in the form of particles instead of a conventional thin film. In addition, the size of the obtained particles can be variously adjusted depending on the application within the range from 1 nm to micron size. Furthermore, composite particles containing GaN nanoparticles in BN particles can be easily synthesized.

  In the method of the present invention, first, a Group IIIB element-containing compound that is soluble in a solvent is prepared as a starting material, and a nitrogen-containing compound such as urea or ammonium salt that is soluble in a solvent is prepared as a nitrogen source, and these are stirred in the solvent. While dissolving. As the solvent, water, alcohol, hydrocarbon solvents (hexane, benzene, toluene, etc.) and the like are used. The dissolution operation may be performed in the atmosphere at room temperature. In addition, it is necessary to select a combination in which the solvent reacts with the raw material and does not completely evaporate. For example, when boric acid is used as a starting material, when boric acid is dissolved and dried only with alcohol, all of the boric acid alkoxide is evaporated. In such a case, water or a substance containing water is used as the solvent. There is a need.

  By arbitrarily changing the molar ratio of the nitrogen-containing compound to the group IIIB element-containing compound of the starting material, the particle size of the generated particles can be controlled. When the amount of the nitrogen-containing compound with respect to the group IIIB element-containing compound is increased, the distance between the group IIIB element-containing compounds increases, so that a smaller particle size can be obtained. For example, when GaN particles are generated by reductive nitridation of a nitrogen-containing compound, the generated GaN particles are combined with GaN particles generated nearby to form GaN particles. At this time, if the distance between the generated GaN particles is increased, the GaN particles are less likely to be combined and can be obtained as GaN particles having a small particle size.

  After the starting material is completely dissolved in the solvent, the resulting transparent liquid is completely dried using an evaporator or a freeze dryer until the mixed powder is free of moisture. At this stage, the starting material is not chemically reacted, and is a lump of a few microns to 1 mm of a uniformly mixed powder.

  The mass of the homogeneous mixture is held as it is in a heating furnace such as a multipurpose high temperature furnace. Since the nitrogen source is supplied from the nitrogen-containing compound, the heating atmosphere may be a reducing atmosphere or an inert atmosphere, and hydrogen, nitrogen, hydrogen + nitrogen, ammonia atmosphere, argon atmosphere, or the like is used. As the heating temperature, a heating temperature and time suitable for causing a nitrogen reaction are selected.

  FIG. 1 shows an example of a heating cycle in the method of the present invention. Heating at about 400 ° C for about 3 hours is for reacting nitrogen-containing compounds such as nitrogen in urea and gallium source, boron source, or indium source. Is decomposed at a high temperature and does not sufficiently react with a gallium source or the like, so that the reaction efficiency is poor and an oxide (such as gallium oxide) may remain.

  In addition, when held at about 300 ° C., which is lower than about 400 ° C., for about 3 hours, the temperature is too low and the reaction of nitrogen of the nitrogen-containing compound and the gallium source is slow. The rate of temperature increase may be about + 5 ° C./min, but if the rate of temperature increase is reduced to about 1 to 0.5 ° C./min, holding at about 400 ° C. for about 3 hours is not necessarily required. Moreover, natural temperature may be sufficient for temperature fall, and it is not necessary to adjust in particular. Since GaN and BN that have just undergone reductive nitridation contain oxygen (particularly BN contains a large amount of oxygen (about 15 wt%)), it is preferable to gradually discharge the GaN or BN by lowering the temperature in a vacuum.

(1) Method for producing BN particles A boron compound such as boric acid that is soluble in a solvent is used as a boron source. In the case of BN particles, the reductive nitriding treatment is preferably about 400 to 1000 ° C. and about 1 to 24 hours. Below this temperature range, the formation of BN particles does not progress much. The obtained BN particles emit light when irradiated with ultraviolet rays. However, when the firing temperature is higher than 1000 ° C., BN particles having good crystallinity and not containing oxygen are generated, so that the emission intensity decreases. When BN particles are synthesized using boric acid or boron oxide as a boron source, turbulent BN is first formed. This stratified BN is continuous with hexagonal BN and is difficult to distinguish. BN with this layered structure contains oxygen, and when heat-treated at a high temperature, hexagonalization proceeds while discharging oxygen. BN particles with strong emission intensity are BN particles with a large amount of oxygen that are heat-treated at a relatively low temperature of 500 to 800 ° C.

(2) Method for producing GaN fine particles A gallium-containing compound such as gallium nitrate which is soluble in a solvent is used as a gallium source. In the case of GaN fine particles, the reduction nitriding treatment is preferably performed at a temperature range of about 400 to 950 ° C. for about 5 to 100 hours. When this temperature is lower than 400 ° C., the nitriding reaction is slow and oxygen remains in the GaN fine particles. When the temperature is higher than 950 ° C., the generated GaN fine particles decompose into Ga and N. The higher the synthesis temperature and the longer the reaction time, the higher crystalline GaN fine particles can be obtained. Usually, when used as a phosphor, a highly crystalline material is desired, but when used for seed crystal growth in a benzene-thermal reaction, a low crystal material is advantageous. According to the method of the present invention, it is possible to synthesize crystalline materials suitable for these applications.

  When In is dissolved in GaN, it can be made smaller than the original band gap of GaN, and the emission wavelength can be controlled. Further, even when GaN is made into nanoparticles and the emission wavelength is shifted to the ultraviolet region due to the quantum size effect, it is possible to emit light in the visible region by dissolving In.

  Conventionally, a gas phase method has been used to produce a Ga—In—N solid solution, but it has been difficult to produce a solid solution because In tends to evaporate at high temperatures. However, in the method of the present invention, a Ga—In—N solid solution can be easily prepared by using, for example, gallium nitrate-indium nitrate-urea as a starting material. At this time, the synthesis temperature can be up to 850 ° C., and the higher the synthesis temperature and the longer the reaction, the higher crystalline Ga—In—N fine particles can be obtained.

(3) Method for producing BN particles including GaN fine particles Generally, there are many defects such as dangling bonds on the surface of the nanoparticles, and excitons are trapped in this and deactivated. However, coating these nanoparticles with a material having a larger band gap causes a quantum confinement effect and increases the emission intensity.

  In the present invention, BN is selected as a material having a larger band gap than GaN, and, for example, by reducing and nitriding using boric acid, gallium nitrate, and a nitrogen-containing compound as a starting material, GaN fine particles are single in hexagonal BN particles. Dispersed and contained BN particles can be produced. By this method, a composite powder in which GaN fine particles having a number average particle diameter of about 1 nm to 1 μm and a solid solution thereof are uniformly dispersed in hexagonal BN is obtained. The size of the GaN fine particles can be ultrafine particles having a number average particle diameter of about 1 nm to 100 nm, and further nanoparticles of about 1 nm to 50 nm.

Example 1
Production of BN particles Boric acid and urea were weighed according to the composition shown in Table 1, completely dissolved in ion-exchanged water, and stirred for 1 hour. Composition 1 is a boric acid: urea molar ratio adjusted to 1: 3, and composition 2 is a boric acid: urea molar ratio adjusted to 1: 6.

  When the solvent was evaporated from 0.5 L of the obtained transparent liquid using an evaporator, 70 g of powder in which boric acid and urea were uniformly mixed was obtained. Then, this mixed powder is placed in an alumina crucible so that 2.5 g of urea is contained (that is, 9.8 g for composition 1, 17 g for composition 2, and 39 g for composition 3), and reduced under the following conditions using a multipurpose high-temperature furnace. As a result of nitriding, 1 g of a sponge-like powder was obtained with composition 1 having a low urea ratio, and 1 g of a white or slightly gray powder having been obtained with compositions 2 and 3 having a high urea ratio.

Reduction condition 1
3 hours at 400 ℃ in hydrogen atmosphere → 12 hours at 500 ℃ → 800 ℃ vacuum (5 × 10 ^-4 Torr or less) 6 hours Reduction condition 2
3 hours at 400 ° C in a hydrogen atmosphere → 12 hours at 800 ° C → 800 ° C vacuum (5 x 10 ^-4 Torr or less) 6 hours Reduction condition 3
400 ℃ for 3 hours in hydrogen atmosphere → 1400 ℃ for 12 hours → 1400 ℃ vacuum (5 × 10 ^-4 Torr or less) for 6 hours

  From the XRD pattern of the obtained sample, a broad BN peak was identified. As a result of TEM observation, the grain boundary could not be identified in the sample synthesized from composition 1, but the sample synthesized from composition 3 is BN fine particles of 200 nm or less, and also confirms nanoparticles of about 50 nm. I was able to. Table 2 shows the oxygen weight contained in the samples obtained by heat-treating compositions 1 and 2 under reducing conditions 2 or 3.

  FIG. 2 shows an XRD chart of a sample obtained by heat-treating composition 3 under reducing conditions 1 to 3. When each was irradiated with ultraviolet light having a wavelength of 365 nm, bright light emission of blue or pale white was observed with the naked eye (visual observation) in the samples prepared under the reducing conditions 1 and 2. The BN fine particles prepared under reducing conditions 1 and 2 had a low degree of hexagonal crystallinity and contained a large amount of oxygen. In contrast, the BN fine particles prepared under reducing condition 3 had high crystallinity and did not contain much oxygen.

This indicates that the strong luminescence observed with BN fine particles is related to the crystallinity and oxygen content of BN fine particles. A similar tendency was also observed in compositions 1 and 2, and the sample synthesized under reducing condition 3 could not confirm strong luminescence with the naked eye, but the sample synthesized under reducing conditions 1 and 2 could confirm strong luminescence. In FIG. 3, the measurement result of the photoluminescence (PL) spectrum of the sample which heat-processed the composition 2 on the reduction conditions 2 is shown (excitation wavelength: 365 nm). Luminescence with a peak near the wavelength of 395 nm was observed.

Example 2
Production of GaN fine particles According to the composition of Table 3, gallium nitrate 6.7 hydrate and urea were weighed, completely dissolved in ion-exchanged water, and stirred for 1 hour. Composition 4 is adjusted so that the molar ratio of gallium nitrate: urea is 1: 2, and composition 5 is adjusted so that the molar ratio of gallium nitrate: urea is 1:10.

  When the solvent was evaporated from 0.2 L of the obtained transparent liquid using an evaporator, 2.6 g of the powder in which gallium nitrate and urea were uniformly mixed and 3.3 g in the composition 5 were obtained. Then, this mixed powder was put in an alumina crucible and subjected to reduction nitridation under the following conditions using a multipurpose high-temperature furnace to obtain about 0.45 g of a free-brown brown or dark brown powder.

Reduction condition 4
400 ° C for 3 hours in a hydrogen atmosphere → 400 ° C vacuum (5 × 10 ^-4 Torr or less) 24 hours reduction condition 5
400 ℃ for 3 hours in hydrogen atmosphere → 800 ° C. for 7 hours → 750 ° C. vacuum (5 × 10 ⁻⁴ Torr or less) 24 hours reduction condition 6
Hydrogen atmosphere 400 ° C 3 hours → 800 ° C 30 hours → 750 ° C vacuum (5 × 10 ^-4 Torr or less) 24 hours reduction condition 7
400 ℃ for 3 hours in hydrogen atmosphere → 800 ° C. for 50 hours → 750 ° C. vacuum (5 × 10 ⁻⁴ Torr or less) for 24 hours

  FIG. 4 shows XRD patterns of Samples 4 and 5 obtained by heat-treating Compositions 4 and 5 under reducing condition 5. From these XRD results, the formation of GaN fine particles was confirmed. FIG. 5 shows TEM observation photographs of the GaN fine particles of Sample 4 and Sample 5. It can be seen that when the amount of urea is large in the starting material, finer GaN nanoparticles were obtained. FIG. 6 shows a PL spectrum measurement result of a sample obtained by heat-treating composition 4 under reducing condition 6 (excitation wavelength: 254 nm). Luminescence with a peak near the wavelength of 390 nm was observed.

Example 3
Production of BN / GaN composite particles According to the composition shown in Table 4, gallium nitrate 6.7 hydrate, boric acid and urea were weighed, completely dissolved in ion-exchanged water, and stirred for 1 hour. Composition 6 is adjusted so that the volume ratio of GaN and BN produced is 10:90, and composition 7 is 30:70.

  When the solvent was evaporated from 0.2 L of the obtained transparent liquid using an evaporator, 5 g of powder in which gallium nitrate, boric acid and urea were uniformly mixed was obtained. This mixed powder was put in an alumina crucible and reduced and nitrided under the following conditions using a multipurpose high-temperature furnace. As a result, a light yellow powder with a composition of about 0.33 g and a composition of about 0.36 g was obtained. It was.

Reduction condition 8
400 ° C for 3 hours in a hydrogen atmosphere → 400 ° C vacuum (5 × 10 ^-4 Torr or less) 24 hours reduction condition 9
400 ℃ for 3 hours in hydrogen atmosphere → 800 ° C. for 7 hours → 750 ° C. vacuum (5 × 10 ⁻⁴ Torr or less) 24 hours reduction condition 10
In a hydrogen atmosphere 400 ° C 3 hours → 800 ° C 30 hours → 750 ° C vacuum (5 × 10 ^-4 Torr or less) 24 hours Reduction condition 11
400 ℃ for 3 hours in hydrogen atmosphere → 800 ° C. for 50 hours → 750 ° C. vacuum (5 × 10 ⁻⁴ Torr or less) for 24 hours

  FIG. 7 shows an XRD pattern of a sample obtained by heat-treating composition 7 under reducing conditions 8-10. Although it is amorphous under the reducing condition 8, it can be seen that the heat treatment under the reducing conditions 9 and 10 consists of only BN and GaN two phases. Further, FIG. 8 shows a TEM observation photograph of Sample 7 obtained by heat-treating Composition 7 under reducing condition 10. It was found that GaN nanoparticles with a particle size of 7-10 nm were monodispersed and uniformly deposited in a matrix composed of hexagonal BN particles. Furthermore, it was found that in the 90 volume% BN / 10 volume% GaN composite particles synthesized from the composition 6 having a high BN content, the dispersed GaN has a finer particle size of 4 to 8 nm. FIG. 9 shows the PL spectrum measurement result of Sample 7 (excitation wavelength: 254 nm). Luminescence with peaks near wavelengths of 350, 390, and 445 nm was observed.

  Nitrides such as GaN and BN having the light emission characteristics obtained by the method of the present invention are phosphors for display and field emission displays such as field emission displays having increased emission quantum efficiency as fine particles, particularly nanoparticles, instead of conventional thin films. -Useful as a light emitter for electronic devices. In addition, by obtaining high purity and low crystalline GaN, it can be applied as a target material for vapor phase synthesis or a seed crystal for hydrothermal synthesis. Furthermore, by obtaining GaN nanoparticles with strong emission intensity whose emission wavelength is blue-shifted by the quantum size effect, it can be applied as an ultraviolet light emitter.

It is a graph which shows an example of the heating cycle in the method of this invention. It is a XRD pattern of the product which heat-processed the composition 3 of Example 1 on reduction conditions 1-3. 2 is a PL spectrum (excitation wavelength: 365 nm) of BN obtained by synthesizing composition 2 of Example 1 under reducing condition 2. FIG. 4 is an XRD pattern of Samples 4 and 5 obtained by heat-treating compositions 4 and 5 of Example 2 under reducing condition 5; 4 is a TEM observation photograph substituting for a drawing of a sample of Example 2. FIG. 4 is a PL spectrum (excitation wavelength: 254 nm) of GaN obtained by synthesizing composition 4 of Example 2 under reducing condition 6. FIG. It is a XRD pattern of the product which heat-processed the composition 7 of Example 2 on reduction conditions 8-10. 5 is a drawing-substituting TEM observation photograph of Sample 7 obtained by heat-treating Composition 7 of Example 2 under reducing condition 10; It is a PL spectrum (excitation wavelength: 254 nm) of Sample 7 of Example 2.

Claims (13)

After dissolving the group IIIB element-containing compound and the nitrogen-containing compound in the solvent, the homogeneous mixture obtained by evaporating the solvent is heated to reduce the group IIIB element-containing compound and nitride the group IIIB element with nitrogen of the nitrogen-containing compound. And a method for synthesizing a group IIIB nitride. 2. The method for synthesizing a group IIIB nitride according to claim 1, wherein the group IIIB nitride is a hexagonal BN, GaN, or Ga—In—N solid solution. The method for synthesizing a group IIIB nitride according to claim 1, wherein the nitrogen-containing compound is urea. The method for synthesizing a group IIIB nitride according to any one of claims 1 to 3, wherein the solvent is water, an alcohol, or a hydrocarbon compound. 2. The method for synthesizing a group IIIB nitride according to claim 1, wherein the group IIIB nitride is fine particles. 2. The method for synthesizing a group IIIB nitride according to claim 1, wherein the group IIIB nitride is a nanoparticle having a number average particle diameter of 1 nm to 50 nm. 2. The method for synthesizing a group IIIB nitride according to claim 1, wherein the group IIIB nitride is micron-sized particles. The method for synthesizing a group IIIB nitride according to any one of claims 5 to 7, wherein the particle size of the generated particles is controlled by adjusting the molar ratio between the group IIIB element-containing compound and the nitrogen-containing compound. The method for synthesizing a group IIIB nitride according to claim 1, wherein the group IIIB nitride is boron nitride (BN) and is a sponge-like lump. 2. The method for synthesizing a group IIIB nitride according to claim 1, wherein the group IIIB nitride is fine particles of a boron layer (BN) of a turbostratic structure type containing oxygen and exhibits fluorescence characteristics. 2. The method for synthesizing a group IIIB nitride according to claim 1, wherein the group IIIB nitride is a GaN nanoparticle and exhibits fluorescence characteristics. The group IIIB nitride according to claim 4, wherein the group IIIB nitride is a composite particle comprising a composite of GaN and hexagonal BN or a composite of Ga-In-N solid solution and hexagonal BN. Synthesis method. The method for synthesizing and producing a group IIIB nitride according to claim 4, wherein the GaN nanoparticles are monodispersed and included in hexagonal BN.

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