CN107364838B - The preparation method of the gallium nitride nano material of iron series element doping - Google Patents
The preparation method of the gallium nitride nano material of iron series element doping Download PDFInfo
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Abstract
The present invention relates to a kind of iron series element doping gallium nitride nano material preparation method, specially heteroatoms iron, cobalt, nickel doped gallium nitride nano material preparation method, belong to Heteroatom doping field of nano material preparation.It is to be dissolved in concentrated nitric acid that it, which is with gallium nitrate salt and nitric acid hetero atom salt, after ammonium hydroxide adjusts PH, is added after complexant reaction and obtains reaction product, reaction product after 450 DEG C of processing again with NH3It is reacted at a temperature of 900-1100 DEG C.The present invention carries out the doping of hetero atom iron-cobalt-nickel by sol-gel method, and further nitridation has been prepared for out the gallium nitride nano particle of different metal doping, can solve the problems such as gallium nitride material Heteroatom doping is difficult to control in traditional handicraft.The present invention at low cost, simple process, reliable in quality in the method for preparing Heteroatom doping gallium nitride nano material.
Description
Technical field
The present invention relates to a kind of iron series element doping gallium nitride nano material preparation method, specially heteroatoms iron,
The preparation method of cobalt, nickel doped gallium nitride nano material, belongs to Heteroatom doping field of nano material preparation.
Background technique
In recent years, the nano material of Heteroatom doping has excellent because of the transmission of its ion and the change of nanostructure
Electricity, light, magnetic physical property, in optics, the numerous areas such as electronics, magnetics, catalysis, biological detection, medicament transport have extensive
Application prospect.Gallium nitride is a kind of direct band gap semiconductor material with wide forbidden band (forbidden bandwidth 3.39eV), gallium nitride, carbonization
The materials such as silicon are referred to as third generation semiconductor material.The gallium nitride of Heteroatom doping has biggish electron mobility, good
Electrical and thermal conductivity, high disruptive field intensity be high, preferable radiation resistance and many characteristics such as high temperature resistant and resistance to chemical corrosion
Thermal conductivity, meanwhile, gallium nitride nano material its luminous efficiency height after Heteroatom doping, in ultraviolet, purple, blue, green luminescent device
Aspect has very big application prospect, is manufacture one of blue light diode and high-power opto-electronic device material the most superior.
Currently, the gallium nitride material of Heteroatom doping prepares inconvenience, physical method is needed to prepare under the high temperature conditions, but right
There are a degree of corrosion and pollutions for environment and equipment, while the gallium nitride nano material of prepared Heteroatom doping is mixed
Miscellaneous ratio is difficult to control, this seriously restricts its performance and is improved.In recent years, people reports chemical method synthesis Heteroatom doping
Gallium nitride nano material, the synthetic method that the gallium nitride nano material of Heteroatom doping is common has: vapour deposition process, molecular beam
Epitaxial growth method, hydride vapour phase epitaxy method etc., but dislocation when the irregular and epitaxial growth of heteroatomic doping is certain
Crystal quality is reduced in degree.
The above technology is all to be used to synthesize the gallium nitride nano material of different Heteroatom dopings using physical method, how to be looked for
It can achieve the preparation method accurately controlled to heteroatomic doping ratio simultaneously to a kind of simple chemical synthesis process to have become
It can be with more excellent performance applications in the key of nano electron device and the field section to solve gallium nitride nano material
Grind the new research direction of worker.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of the gallium nitride nano material of iron series element doping, features
It is further to be nitrogenized after calcining, direct nitridation method is prepared for difference by sol-gel method adjustment and control system pH and coordination situation
The gallium nitride nano material of Heteroatom doping can solve in traditional handicraft gallium nitride material Heteroatom doping and be difficult to control etc. and asks
Topic.The present invention at low cost, simple process, reliable in quality in the method for preparing Heteroatom doping gallium nitride nano material.
The preparation method of the gallium nitride nano material of iron series element doping provided by the invention is with gallium nitrate salt and nitric acid
Hetero atom salt is to be dissolved in concentrated nitric acid, after ammonium hydroxide adjusts pH, obtains reaction product, reaction product after complexant reaction is added
In 450 DEG C processing after again with NH3It is reacted at a temperature of 900-1100 DEG C.
Iron provided by the invention, cobalt, the doping of ferronickel series elements the preparation method of gallium nitride nano material include the steps that
Are as follows:
1) nitrate of gallium nitrate hydrate and heteroatoms iron, cobalt, nickel is dissolved in concentrated nitric acid, acquired solution ammonium hydroxide tune
Section pH is 7.5-8.2；After mixing evenly, it is warming up to 70-80 DEG C, citric acid is added, after being completely dissolved, continues heating 2-4 h and obtains
To clear gum object；
2) under air conditions, gained clear gum object is placed among the crucible of Muffle furnace, temperature programming to 400-450
DEG C, it heats 4-6 hours, naturally cools to room temperature, obtain grey coralliform solid；Obtained solid is transferred in tube furnace, is taken out true
Sky, temperature programming are passed through the NH of 100-300 sccm to 900-1100 DEG C3, after maintaining 2-4 hours, it is cooled under argon gas protection
Room temperature obtains faint yellow product.
The iron series element is iron, cobalt, nickel, and the content of hetero atom nitrate is the 1-6% of gallium nitrate.
The amount of citric acid described in step 1) need to be coordinated gallium ion and hetero atom ion completely.
400-450 DEG C of temperature programming described in step 2 is: 2 DEG C/min, starting to warm up from 20 DEG C of room temperature, heating 215
min。
Temperature programming described in step 2 is in 900-1100 DEG C, and the temperature programming is 5 DEG C/minute, since 20 DEG C
Heating, heat up 176-216 min.Vacuum degree described in step 2 is -0.1Mpa.
The preparation method of the gallium nitride nano material of iron series element doping provided by the invention is with gallium nitrate salt and nitric acid
Hetero atom salt is to be dissolved in concentrated nitric acid, after ammonium hydroxide adjusts p H, obtains reaction product after complexant reaction is added, reaction produces
Object in 400-450 DEG C processing after again with NH3It is reacted at a temperature of 900-1100 DEG C.Its main feature is that solidifying by colloidal sol-
Glue method carries out the doping of hetero atom iron-cobalt-nickel, further nitrogenizes, and has been prepared for out the gallium nitride nano particle of different metal doping,
It can solve the problems such as gallium nitride material Heteroatom doping is difficult to control in traditional handicraft.The present invention is preparing Heteroatom doping nitrogen
Change at low cost, simple process in the method for gallium nano material, reliable in quality.
Detailed description of the invention
Fig. 1 is the SEM figure of Fe2O3 doping gallium nitride nano material prepared by embodiment 1.
Fig. 2 is the SEM figure of cobalt doped gallium nitride nano material prepared by embodiment 1.
Fig. 3 is the SEM figure of nickel doped gallium nitride nano material prepared by embodiment 1.
Fig. 4 be embodiment 1 prepared by iron, cobalt, nickel doped gallium nitride nano material XRD diagram.
Fig. 5 be embodiment 1 prepared by iron, cobalt, nickel doped gallium nitride nano material ultraviolet-visible absorption spectroscopy.
Fig. 6 be embodiment 1 prepared by iron, cobalt, nickel doped gallium nitride nano material Raman spectrum.
Specific embodiment
Embodiment 1
25.57 grams of gallium nitrate hydrate (analysis pure) and 1% 0.40 gram of ferric nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 186 min, and temperature programming is passed through to 950 DEG C
The NH of 100 sccm3, after maintaining 3 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 16.6 g.
Embodiment 2
25.57 grams of gallium nitrate hydrate (analysis pure) and 1% 0.29 gram of cobalt nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 186 min, and temperature programming is passed through to 950 DEG C
The NH of 100 sccm3, after maintaining 3 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 3.75 g.
Embodiment 3
25.57 grams of gallium nitrate hydrate (analysis pure) and 1% 0.29 gram of nickel nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 186 min, and temperature programming is passed through to 950 DEG C
The NH of 100 sccm3, after maintaining 3 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 2.96 g.
Embodiment 4
25.57 grams of gallium nitrate hydrate (analysis pure) and 6% 2.40 grams of ferric nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 186 min, and temperature programming is passed through to 950 DEG C
The NH of 100 sccm3, after maintaining 3 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 4.21 g.
Embodiment 5
25.57 grams of gallium nitrate hydrate (analysis pure) and 6% 1.74 grams of nickel nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 186 min, and temperature programming is passed through to 950 DEG C
The NH of 100 sccm3, after maintaining 3 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 4.20 g.
Embodiment 6
25.57 grams of gallium nitrate hydrate (analysis pure) and 6% 1.74 grams of nickel nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 186 min, and temperature programming is passed through to 950 DEG C
The NH of 100 sccm3, after maintaining 3 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 3.56 g.
Embodiment 7
25.57 grams of gallium nitrate hydrate (analysis pure) and 3% 1.20 grams of ferric nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 186 min, and temperature programming is passed through to 950 DEG C
The NH of 100 sccm3, after maintaining 3 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 2.65 g.
Embodiment 8
25.57 grams of gallium nitrate hydrate (analysis pure) and 3% 0.87 gram of ferric nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 186 min, and temperature programming is passed through to 950 DEG C
The NH of 100 sccm3, after maintaining 3 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 3.40 g.
Embodiment 9
25.57 grams of gallium nitrate hydrate (analysis pure) and 3% 0.87 gram of nickel nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 196 min, and temperature programming is passed through to 950 DEG C
The NH of 100 sccm3, after maintaining 3 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 3.61 g.
Embodiment 10
25.57 grams of gallium nitrate hydrate (analysis pure) and 1% 0.40 gram of ferric nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 6 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 176 min, and temperature programming is passed through to 900 DEG C
The NH of 200 sccm3, after maintaining 4 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 3.32 g.
Embodiment 11
25.57 grams of gallium nitrate hydrate (analysis pure) and 1% 0.40 gram of ferric nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 4 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 198 min, and temperature programming is passed through to 1000 DEG C
The NH of 100 sccm3, after maintaining 2 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 4.50 g.
Embodiment 12
25.57 grams of gallium nitrate hydrate (analysis pure) and 1% 0.40 gram of ferric nitrate hydrate (analyzing pure) is taken to exist respectively
It is dissolved in concentrated nitric acid in 100 mL beakers；Under magnetic agitation, acquired solution is adjusted into pH with the ammonium hydroxide of 35-37% concentration dropwise,
PH value to system is 7.6, consumes 20 mL of ammonium hydroxide.After mixing evenly, 80 DEG C are heated to, and 3 g citric acids are added, it is complete
After fully dissolved, continues 80 DEG C of 2 h of holding, obtain clear gum object；Gained clear gum object is further arranged in the earthenware of Muffle furnace
It among crucible, with the heating rate of 2 DEG C/min, is started to warm up from 20 DEG C of room temperature, heat up 215 min, and temperature programming adds to 450 DEG C
Heat 4 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, be evacuated to-
0.1 MPa is started to warm up with the heating rate of 5 DEG C/min from 20 DEG C, and heat up 198 min, and temperature programming is passed through to 1000 DEG C
The NH of 300 sccm3, after maintaining 3 hours, it is cooled to room temperature under argon gas protection, obtains the faint yellow product of 3.62 g.
Claims (4)
1. a kind of preparation method of the gallium nitride nano material of iron series element doping, it is characterised in that it is by following step:
1) gallium nitrate hydrate and iron, cobalt, nickel nitrate are dissolved in concentrated nitric acid, it is 7.5- that acquired solution, which adjusts pH with ammonium hydroxide,
8.2；After mixing evenly, it is warming up to 70-80 DEG C, citric acid is added, after being completely dissolved, continues heating 2-4 h and obtains clear gum
Object；
The amount of the citric acid need to be coordinated gallium ion and hetero atom ion completely；
2) under air conditions, gained clear gum object is placed among the crucible of Muffle furnace, temperature programming to 400-450 DEG C,
Heating 4-6 hours, naturally cools to room temperature, obtains grey coralliform solid；Obtained solid is transferred in tube furnace, is vacuumized,
Temperature programming is passed through the NH of 100-300 sccm to 900-1100 DEG C3, after maintaining 2-4 hours, room is cooled under argon gas protection
Temperature obtains faint yellow product；
The 400-450 DEG C of temperature programming is: 2 DEG C/min, starting to warm up from 20 DEG C of room temperature, heat up 215 min.
2. preparation method according to claim 1, it is characterised in that the iron, cobalt, nickel nitrate and gallium nitrate rub
You are than being 1-6%.
3. preparation method according to claim 1, it is characterised in that temperature programming described in step 2 is to 900-1100 DEG C
In, the temperature programming is 5 DEG C/minute, is started to warm up from 20 DEG C, and heat up 176-216 min.
4. preparation method according to claim 1, it is characterised in that vacuum degree described in step 2 is -0.1Mpa.
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| KR20080004236A (en) * | 2006-07-05 | 2008-01-09 | 주식회사 엘지화학 | Method for preparing of spherical colloidal crystal with opalescence effect |
| CN104449689A (en) * | 2014-12-14 | 2015-03-25 | 励春亚 | Preparation method of rare-earth doped GaN material |
| CN106824242A (en) * | 2017-01-19 | 2017-06-13 | 京东方科技集团股份有限公司 | The preparation method and material for air purification of a kind of material for air purification |
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Patent Citations (6)
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|---|---|---|---|---|
| JP2003124518A (en) * | 2002-09-17 | 2003-04-25 | Seiwa Electric Mfg Co Ltd | Gallium nitride semiconductor light emitting element and its manufacturing method |
| CN1517448A (en) * | 2003-01-13 | 2004-08-04 | 中国科学院长春光学精密机械与物理研 | Gallium nitride nanometer polycrystal film made by sol-gel method |
| KR20080004236A (en) * | 2006-07-05 | 2008-01-09 | 주식회사 엘지화학 | Method for preparing of spherical colloidal crystal with opalescence effect |
| CN1944268A (en) * | 2006-10-25 | 2007-04-11 | 国家纳米技术与工程研究院 | Method for preparing gallium nitride nano crystal using sol-gel method |
| CN104449689A (en) * | 2014-12-14 | 2015-03-25 | 励春亚 | Preparation method of rare-earth doped GaN material |
| CN106824242A (en) * | 2017-01-19 | 2017-06-13 | 京东方科技集团股份有限公司 | The preparation method and material for air purification of a kind of material for air purification |
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| 稀土掺杂氮化镓纳米粉溶胶-凝胶制备及发光机理研究;张璐;《西北大学硕士学位论文》;20110831;第33-34页 * |
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