CN108913133A - A kind of preparation method of deep ultraviolet excitated type nano-phosphor - Google Patents
A kind of preparation method of deep ultraviolet excitated type nano-phosphor Download PDFInfo
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- CN108913133A CN108913133A CN201810772532.5A CN201810772532A CN108913133A CN 108913133 A CN108913133 A CN 108913133A CN 201810772532 A CN201810772532 A CN 201810772532A CN 108913133 A CN108913133 A CN 108913133A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7736—Vanadates; Chromates; Molybdates; Tungstates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7708—Vanadates; Chromates; Molybdates; Tungstates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
- C09K11/7751—Vanadates; Chromates; Molybdates; Tungstates
Abstract
The invention discloses a kind of preparation methods of deep ultraviolet excitated type nano-phosphor, use two phase process first, enormously simplify preparation process.Secondly, increasing phase interface using rotating packed-bed reactor for the mechanism for cooperating two phase process to react at phase interface.Reinforce mass transfer simultaneously, ensure that good repeatability between the uniformity of product and different batches of product, and substantially reduces reaction required time.And replace toluene as solvent using environmentally protective high boiling atoleine, toxicity is low and is not easy to evaporate into external environment.Convenience is created for the development of optimization experimental implementation and extensive synthesis monodisperse calcium molybdate fluorescent nano material.
Description
Technical field
The invention belongs to chemical industry, material and photonics crossing domain, be related to it is a kind of using hypergravity reaction reinforcement technique i.e.
Rotating packed-bed reactor is prepared using calcium molybdate as the method for the deep ultraviolet excitated type nano-phosphor of matrix.
Background technique
As energy-efficient new generation of green lighting source, in recent years, the technology of solid-state semiconductor LED chip develops
Rapidly, from blue light (450-480nm) to ultraviolet light (380-420nm), the LED chip of different wave length is developed successively.It is deep
Ultraviolet light (200-350nm) energy is very high, and is entirely free of visible light, is conducive to the adjusting of color quasi-, is more suitable for high-power height
Brightness LED chip.The LED chip minimal wave length reported at present is 210nm, and the 280nm of Luminus Devices company exploitation
Deep ultraviolet LED chip has been realized in volume production commercialization.
In order to promote the transparency that the light emission rate of LED needs to increase packaging plastic, it is therefore necessary to improve and develop fluorescent powder and exist
Stabilization in organic solvent is without scattering suspension performance.It is this however currently, most of fluorescent powders contain the particle of micron size
The particle of micron size has stronger scattering properties.It can be obtained based on Mie theory for being less than the particle of 50nm
Without scattering properties.Therefore, it is necessary to nano grade inorganic fluorescent powders.The synthetic method of many high-temperature solids has now been developed to make
Make nano-phosphor.But this inorganic nano fluorophor is easy to assemble in organic solvent, it is therefore desirable to manufacture inorganic nano
The stable suspension of fluorophor.And the primary synthetic methods without scattering suspension of calcium molybdate fluorescent powder are that will use oleic acid at present
Radical ion (OA-) is by calcium, sodium and rare earth ion from being transferred in toluene phase in water phase.Equally make molybdenum acid ion and four octyl ammoniums
(TOA) cation complex is transferred to toluene phase.Contain calcium oleate (europium, enuatrol) and TOA-MoO for two kinds4The toluene of complex compound
Solution mixing.Then mixture is transferred in autoclave and is reacted.Its key reaction formula is：
Ca2++MoO4 2-→CaMoO4
This method can prepare that particle size is small and the nano-phosphor of favorable dispersibility.But this method there is also
Some disadvantages：
1, toluene is a kind of volatile and is hazardous to the human body, is easy the organic solvent polluted the environment, to preparation
The safety of personnel causes centainly to threaten.
2, without effectively mixing mass transfer means, product repeatability and the uniformity are bad when batch production.Quality is not easy to
Control.
3, it is longer the time required to reaction, and the cumbersome multiple extraction step of needs of reaction step.Production cycle is long, cost compared with
It is high.
Due to disadvantage mentioned above, there is an urgent need to study a kind of green, the easy dispersion nano-phosphor that is simply amplified by people
Preparation process.
Hypergravity refers to suffered by substance, its acceleration is made to be greater than terrestrial gravitation acceleration (9.8m/s2) power.Super
Under gravity environment, due to the presence of huge acceleration, under violent collision liquid be split into micron even nanoscale film,
Silk and droplet generate phase interface that is huge and quickly updating between incompatible two-phase originally.The phase interface of increase makes
The reaction of generation is easier to carry out at phase interface, keeps the composite character time of molecule shorter than nucleation induction required time, energy while shape
At a large amount of nucleus.And phase interface, which quickly updates, can hinder nucleus growth to ultimately generate small size nano particle.Hypergravity equipment
Hypergravity reaction environment is provided for experiment, and rotary packed bed is a kind of typical hypergravity equipment.Molecule diffusion and alternate biography
Matter process can greatly be reinforced, and microcosmic mixing and mass transport process are greatly strengthened
Summary of the invention
The present invention uses two phase process first, enormously simplifies preparation process.Secondly, in order to cooperate two phase process at phase interface
The mechanism of reaction increases phase interface using rotating packed-bed reactor.Reinforce mass transfer simultaneously, ensure that the uniformity and not of product
With repeatability good between batch products, and substantially reduce reaction required time.And using environmentally protective high boiling
Atoleine replaces toluene as solvent, and toxicity is low and is not easy to evaporate into external environment.For optimization experimental implementation and greatly
The development of scale synthesis monodisperse calcium molybdate fluorescent nano material creates convenience.
The technical solution adopted by the present invention is a kind of preparation method of deep ultraviolet excitated type nano-phosphor, the preparation method
Steps are as follows：
Total amount 4mmol calcium nitrate, europium nitrate and sodium nitrate are dissolved in 20ml water by S1；The wherein molal quantity phase of sodium and europium
Together.Europium shared molar ratio in three kinds of calcium, europium and sodium cations is 0~10%.Excessive enuatrol, 10ml oleic acid and 10ml is added
Oleyl amine；Atoleine is added, the volume of atoleine is twice of water volume, stirs 1 hour, obtains mixing liquid.
The ammonium molybdate of 0.57mmol will be dissolved in 20ml water by S2.Ammonium molybdate solution is added in the mixing liquid in S1,
Obtain mixed solution.
The finally obtained mixed solution of S2 is added in internal-circulation type rotary packed bed S3.At 80 DEG C of temperature, internal-circulation type
Under rotary packed bed revolving speed 1000r/min~2000r/min, reacts 1~6 hour, obtain reaction solution.
S4 takes out reaction solution and is cooled to room temperature.It is centrifugated out upconversion fluorescence nano material and uses dehydrated alcohol
After cleaning repeatedly, it is placed in air at room temperature drying, obtains solid nano fluorescent powder.
Europium nitrate can be replaced with dysprosium nitrate or thulium nitrate.
The required source chemicals for realizing above-mentioned nano-phosphor material synthesis method include：Commercial rare earth nitrades (nitre
Sour europium, terbium nitrate, dysprosium nitrate), calcium nitrate, sodium nitrate, enuatrol, ammonium molybdate, oleic acid, oleyl amine, atoleine, dehydrated alcohol.
Required experimental provision equipment includes：Beaker, magnetic stirring apparatus, internal-circulation type rotary packed bed, cryogenic thermostat reactive bath technique, centrifugation
Machine (centrifuge tube), ultrasonic cleaner.
Detailed description of the invention
Fig. 1 is transmission electron microscope (TEM) photo of the deep ultraviolet excitation nano fluorescent powder of the method for the present invention preparation.
Fig. 2 is X diffraction (XRD) spectrum of the deep ultraviolet excitation nano fluorescent powder of the method for the present invention preparation.
Fig. 3 be the method for the present invention preparation europium adulterate deep ultraviolet excitation nano fluorescent powder in 260nm, 280nm, 300nm and
Fluorescence emission spectrum under 320nm laser excitation.
Fig. 4 be the terbium doped deep ultraviolet excitation nano fluorescent powder of the method for the present invention preparation in 260nm, 280nm, 300nm and
Fluorescence emission spectrum under 320nm laser excitation.
Fig. 5 be the dysprosium doped deep ultraviolet excitation nano fluorescent powder of the method for the present invention preparation in 260nm, 280nm, 300nm and
Fluorescence emission spectrum under 320nm laser excitation.
Specific embodiment
Embodiment 1
0.40mmol europium nitrate, 0.40mmol sodium nitrate are weighed respectively, and 3.20mmol calcium nitrate and 8.8mol enuatrol are put
Enter in 250 milliliters of beaker.20 ml deionized waters, 80 milliliters of liquid paraffin, 10 milliliters of oleic acid and 10 milliliters of oleyl amines are added, it will
Solution stirs 1 hour, forms rice white lotion.0.57mol ammonium molybdate is weighed to be dissolved in 20 milliliters of water.By lotion and ammonium molybdate
Internal-circulation type rotary packed bed is all added in solution, keeps making nano-phosphor in 6 hours under the conditions of 80 DEG C, revolving speed 2000r/min
It generates.It takes out reaction solution to be cooled to room temperature, it is later anti-with dehydrated alcohol to be centrifugated out deep ultraviolet excitation nano fluorescent material
Multiple cleaning is placed in air at room temperature drying, can obtain solid deep ultraviolet excitation nano fluorescent material.
Embodiment 2
0.20mmol europium nitrate, 0.20mmol sodium nitrate are weighed respectively, and 3.60mmol calcium nitrate and 8.8mol enuatrol are put
Enter in 250 milliliters of beaker.20 ml deionized waters, 80 milliliters of liquid paraffin, 10 milliliters of oleic acid and 10 milliliters of oleyl amines are added, it will
Solution stirs 1 hour, forms rice white lotion.0.57mol ammonium molybdate is weighed to be dissolved in 20ml water.Lotion and ammonium molybdate is molten
Internal-circulation type rotary packed bed is all added in liquid, keeps making within 3 hours nano-phosphor raw under the conditions of 80 DEG C, revolving speed 1500r/min
At.It takes out reaction solution to be cooled to room temperature, be centrifugated out after deep ultraviolet excitation nano fluorescent material with dehydrated alcohol repeatedly
Cleaning is placed in air at room temperature drying, can obtain solid deep ultraviolet excitation nano fluorescent material.
Embodiment 3
0.04mmol europium nitrate, 0.04mmol sodium nitrate are weighed respectively, and 3.92mmol calcium nitrate and 8.8mol enuatrol are put
Enter in 250 milliliters of beaker.20 ml deionized waters, 80 milliliters of liquid paraffin, 10 milliliters of oleic acid and 10 milliliters of oleyl amines are added, it will
Solution stirs 1 hour, forms rice white lotion.0.57mol ammonium molybdate is weighed to be dissolved in 20 milliliters of water.By lotion and ammonium molybdate
Internal-circulation type rotary packed bed is all added in solution, keeps making nano-phosphor in 1 hour under the conditions of 80 DEG C, revolving speed 1000r/min
It generates.It takes out reaction solution to be cooled to room temperature, it is later anti-with dehydrated alcohol to be centrifugated out deep ultraviolet excitation nano fluorescent material
Multiple cleaning is placed in air at room temperature drying, can obtain solid deep ultraviolet excitation nano fluorescent material.
Embodiment 4
0.40mmol terbium nitrate, 0.40mmol sodium nitrate are weighed respectively, and 3.20mmol calcium nitrate and 8.8mol enuatrol are put
Enter in 250 milliliters of beaker.20 ml deionized waters, 80 milliliters of liquid paraffin, 10 milliliters of oleic acid and 10 milliliters of oleyl amines are added, it will
Solution stirs 1 hour, forms rice white lotion.0.57mol ammonium molybdate is weighed to be dissolved in 20 milliliters of water.By lotion and ammonium molybdate
Internal-circulation type rotary packed bed is all added in solution, keeps making nano-phosphor in 6 hours under the conditions of 80 DEG C, revolving speed 2000r/min
It generates.It takes out reaction solution to be cooled to room temperature, it is later anti-with dehydrated alcohol to be centrifugated out deep ultraviolet excitation nano fluorescent material
Multiple cleaning is placed in air at room temperature drying, can obtain solid deep ultraviolet excitation nano fluorescent material.
Embodiment 5
0.20mmol terbium nitrate, 0.20mmol sodium nitrate are weighed respectively, and 2.60mmol calcium nitrate and 8.8mol enuatrol are put
Enter in 250 milliliters of beaker.20 ml deionized waters, 80 milliliters of liquid paraffin, 10 milliliters of oleic acid and 10 milliliters of oleyl amines are added, it will
Solution stirs 1 hour, forms rice white lotion.0.57mol ammonium molybdate is weighed to be dissolved in 20ml water.Lotion and ammonium molybdate is molten
Internal-circulation type rotary packed bed is all added in liquid, keeps making within 3 hours nano-phosphor raw under the conditions of 80 DEG C, revolving speed 1500r/min
At.It takes out reaction solution to be cooled to room temperature, be centrifugated out after deep ultraviolet excitation nano fluorescent material with dehydrated alcohol repeatedly
Cleaning is placed in air at room temperature drying, can obtain solid deep ultraviolet excitation nano fluorescent material.
Embodiment 6
0.04mmol terbium nitrate, 0.04mmol sodium nitrate are weighed respectively, and 3.92mmol calcium nitrate and 8.8mol enuatrol are put
Enter in 250 milliliters of beaker.20 ml deionized waters, 80 milliliters of liquid paraffin, 10 milliliters of oleic acid and 10 milliliters of oleyl amines are added, it will
Solution stirs 1 hour, forms rice white lotion.0.57mol ammonium molybdate is weighed to be dissolved in 20 milliliters of water.By lotion and ammonium molybdate
Internal-circulation type rotary packed bed is all added in solution, keeps making nano-phosphor in 1 hour under the conditions of 80 DEG C, revolving speed 1000r/min
It generates.It takes out reaction solution to be cooled to room temperature, it is later anti-with dehydrated alcohol to be centrifugated out deep ultraviolet excitation nano fluorescent material
Multiple cleaning is placed in air at room temperature drying, can obtain solid deep ultraviolet excitation nano fluorescent material.
Embodiment 7
0.40mmol dysprosium nitrate, 0.40mmol sodium nitrate are weighed respectively, and 3.20mmol calcium nitrate and 8.8mol enuatrol are put
Enter in 250 milliliters of beaker.20 ml deionized waters, 80 milliliters of liquid paraffin, 10 milliliters of oleic acid and 10 milliliters of oleyl amines are added, it will
Solution stirs 1 hour, forms rice white lotion.0.57mol ammonium molybdate is weighed to be dissolved in 20 milliliters of water.By lotion and ammonium molybdate
Internal-circulation type rotary packed bed is all added in solution, keeps making nano-phosphor in 6 hours under the conditions of 80 DEG C, revolving speed 2000r/min
It generates.It takes out reaction solution to be cooled to room temperature, it is later anti-with dehydrated alcohol to be centrifugated out deep ultraviolet excitation nano fluorescent material
Multiple cleaning is placed in air at room temperature drying, can obtain solid deep ultraviolet excitation nano fluorescent material.
Embodiment 8
0.20mmol dysprosium nitrate, 0.20mmol sodium nitrate are weighed respectively, and 3.60mmol calcium nitrate and 8.8mol enuatrol are put
Enter in 250 milliliters of beaker.20 ml deionized waters, 80 milliliters of liquid paraffin, 10 milliliters of oleic acid and 10 milliliters of oleyl amines are added, it will
Solution stirs 1 hour, forms rice white lotion.0.57mol ammonium molybdate is weighed to be dissolved in 20ml water.Lotion and ammonium molybdate is molten
Internal-circulation type rotary packed bed is all added in liquid, keeps making within 3 hours nano-phosphor raw under the conditions of 80 DEG C, revolving speed 1500r/min
At.It takes out reaction solution to be cooled to room temperature, be centrifugated out after deep ultraviolet excitation nano fluorescent material with dehydrated alcohol repeatedly
Cleaning is placed in air at room temperature drying, can obtain solid deep ultraviolet excitation nano fluorescent material.
Embodiment 9
0.04mmol dysprosium nitrate, 0.04mmol sodium nitrate are weighed respectively, and 3.92mmol calcium nitrate and 8.8mol enuatrol are put
Enter in 250 milliliters of beaker.20 ml deionized waters, 80 milliliters of liquid paraffin, 10 milliliters of oleic acid and 10 milliliters of oleyl amines are added, it will
Solution stirs 1 hour, forms rice white lotion.0.57mol ammonium molybdate is weighed to be dissolved in 20 milliliters of water.By lotion and ammonium molybdate
Internal-circulation type rotary packed bed is all added in solution, keeps making nano-phosphor in 1 hour under the conditions of 80 DEG C, revolving speed 1000r/min
It generates.It takes out reaction solution to be cooled to room temperature, it is later anti-with dehydrated alcohol to be centrifugated out deep ultraviolet excitation nano fluorescent material
Multiple cleaning is placed in air at room temperature drying, can obtain solid deep ultraviolet excitation nano fluorescent material.
The content of present invention is described further below.
Fig. 1 show based on the method for the present invention prepare burst of ultraviolel nano-luminescent material be peanut shaped major diameter be about 20nm,
Minor axis is about 1.5nm.
What Fig. 2 showed to prepare based on the method for the present invention is tetragonal phase calcium molybdate.
Fig. 3 shows the europium doping deep ultraviolet excitation nano fluorescent powder prepared based on the method for the present invention in 260-320nm laser
The lower feux rouges that can issue 615nm of light excitation.
Fig. 4 shows the terbium doped deep ultraviolet excitation nano fluorescent powder prepared based on the method for the present invention in 260-320nm laser
The lower green light that can issue 547nm of light excitation.
Fig. 5 shows the dysprosium doped deep ultraviolet excitation nano fluorescent powder prepared based on the method for the present invention in 260-320nm laser
The lower yellow light that can issue 573nm of light excitation.
Claims (2)
1. a kind of preparation method of deep ultraviolet excitated type nano-phosphor, it is characterised in that：Steps are as follows for the preparation method：
Total amount 4mmol calcium nitrate, europium nitrate and sodium nitrate are dissolved in 20ml water by S1；Wherein sodium is identical as the molal quantity of europium；Europium
Shared molar ratio is 0~10% in three kinds of calcium, europium and sodium cations；Excessive enuatrol, 10ml oleic acid and 10ml oleyl amine is added；
Atoleine is added, the volume of atoleine is twice of water volume, stirs 1 hour, obtains mixing liquid；
The ammonium molybdate of 0.57mmol will be dissolved in 20ml water by S2；Ammonium molybdate solution is added in the mixing liquid in S1, is obtained
Mixed solution；
The finally obtained mixed solution of S2 is added in internal-circulation type rotary packed bed S3；At 80 DEG C of temperature, internal-circulation type rotates
Under packed bed revolving speed 1000r/min~2000r/min, reacts 1~6 hour, obtain reaction solution；
S4 takes out reaction solution and is cooled to room temperature；Be centrifugated out upconversion fluorescence nano material and with dehydrated alcohol repeatedly
After cleaning, it is placed in air at room temperature drying, obtains solid nano fluorescent powder.
2. a kind of preparation method of deep ultraviolet excitated type nano-phosphor according to claim 1, it is characterised in that：Nitric acid
Europium can be replaced with dysprosium nitrate or thulium nitrate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109580482A (en) * | 2018-12-04 | 2019-04-05 | 华北电力大学 | Microstate observation device and its method in a kind of reinforced by nanoparticles mass-transfer progress |
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| CN107033895A (en) * | 2017-04-09 | 2017-08-11 | 北京化工大学 | A kind of preparation method of rear-earth-doped oxide nano-sized upconversion phosphor |
| CN107814409A (en) * | 2017-10-27 | 2018-03-20 | 华南理工大学 | A kind of green ultrasound synthesis different structure CsPbBr3The method of nanocrystal |
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2018
- 2018-07-13 CN CN201810772532.5A patent/CN108913133A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033895A (en) * | 2017-04-09 | 2017-08-11 | 北京化工大学 | A kind of preparation method of rear-earth-doped oxide nano-sized upconversion phosphor |
| CN107814409A (en) * | 2017-10-27 | 2018-03-20 | 华南理工大学 | A kind of green ultrasound synthesis different structure CsPbBr3The method of nanocrystal |
Non-Patent Citations (1)
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| MYEONG-JIN KIM ET AL.: "Synthesis and optical properties of CaMoO4:Eu3+, Na+ nanophosphors and a transparent CaMoO4:Eu3+, Na+ suspension", 《OPTICAL MATERIALS》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109580482A (en) * | 2018-12-04 | 2019-04-05 | 华北电力大学 | Microstate observation device and its method in a kind of reinforced by nanoparticles mass-transfer progress |
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