CN106947481B - A kind of red Illuminant nanometer fluorescent powder of europium ion activation, preparation method and application - Google Patents
A kind of red Illuminant nanometer fluorescent powder of europium ion activation, preparation method and application Download PDFInfo
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- CN106947481B CN106947481B CN201710196167.3A CN201710196167A CN106947481B CN 106947481 B CN106947481 B CN 106947481B CN 201710196167 A CN201710196167 A CN 201710196167A CN 106947481 B CN106947481 B CN 106947481B
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- 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
- C09K11/7737—Phosphates
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- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
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Abstract
The invention discloses a kind of red Illuminant nanometer fluorescent powder of europium ion activation, preparation method and application, materials chemistry formula is Bi1‑ xEuxSbP4O14, x is trivalent europium ion Eu3+Replace Bi3+The molar ratio of ion, value range are 0.001≤x≤0.25.Red Illuminant nanometer fluorescent powder of the invention issues pure feux rouges of the dominant wavelength at 614 nanometers under ultraviolet, near ultraviolet and blue light excitation, it can be applied in various illuminations and display device using ultraviolet, near ultraviolet and blue light as excitaton source, with modulated light source colour temperature and improve colour rendering index.Red Illuminant nanometer fluorescent powder grain of the invention is tiny, granule size is uniform, it can be mixed with blue, green emitting phosphor, apply and be packaged in outside InGaN diode, prepare the LED of capable of emitting warm white；Matrix stablizes corrosion-resistant, luminous efficiency height, Nonpoisonous, non-environmental-pollution；Its preparation process is highly susceptible to operation and industrialized production.
Description
Technical field
The present invention relates to a kind of red Illuminant nanometer fluorescent powders of europium ion activation, preparation method and application, belong to inorganic hair
Luminescent material technical field.
Background technique
White light LEDs are a kind of novel illuminating devices, are the green light sources attracted attention by scientific research and market 21 century, have
Boundless application market prospect.White light LEDs have power consumption small (the 1/8 of incandescent lamp bulb, the 1/2 of fluorescent lamp bulb), fever
Measure low, reaction speed is fast, small in size, service life long (tens of thousands of hours be fluorescent lamp 10 times), can planar package the advantages that, easy exploiting
It is that the potentiality product that traditional lighting utensil is substituted in coming 10 years is had an optimistic view of by industry at light and short product.Current white light LEDs
In development process, realize that white light LEDs have become using 350~410 nanometers of InGaN tube core excitation three primary colors fluorescent powders of black light
One of the hot spot that the field is researched and developed in the world at present, it is considered to be White-light LED illumination of new generation is dominated.In preparation the type
In White-light LED illumination device, red, blue, green three primary colors fluorescent powder plays very important effect, therefore, develop it is new and effective,
The good red of thermal stability, green and blue fluorescent powder are the key that improve White-light LED illumination device luminous mass.
Among three primary colors fluorescent powder, compared with blue and green emitting phosphor, service efficiency needs to be mentioned red fluorescence powder
Height, in the red fluorescence powder developed at present, trivalent europium Eu3+The red fluorescence powder of ion excitation is most important one kind, by
It is extensively studied and is applied to luminescence display field, but Eu3+The absorption of itself has the structure of doped substrate and its important
Dependence, therefore research and develop new matrix, realize trivalent europium Eu3+Ion effectively shines, and receives the extensive concern of researcher.
In addition, the existing red fluorescence powder that can be effectively excited by black light is fewer, and granularity is not suitable for greatly coating, and stability is not
Height, coloration is impure, can also generate the toxic gases such as sulfide under uv irradiation, cause damages to environment, make trouble,
The cost that producing process is spent is also higher.Therefore the good red fluorescence powder of research performance not only has certain theory significance, more
With important practical application meaning.
Summary of the invention:
It can be by black light in view of the above-mentioned problems of the prior art, the first purpose of the invention is to provide one kind
Effectively excitation, granularity is small, and stability is good, luminous mass is high and the red Illuminant nanometer fluorescent powder of free of contamination europium ion activation, this
The another object of invention is to provide the preparation method of the red Illuminant nanometer fluorescent powder of above-mentioned europium ion activation, guarantees to operate letter
Single, at low cost and favorable repeatability, third object of the present invention are that the red Illuminant nanometer for providing above-mentioned europium ion activation is glimmering
The application of light powder.
To achieve the above objectives, the technical solution adopted by the present invention is that: a kind of red Illuminant nanometer fluorescence of europium ion activation
Powder, chemical formula Bi1-xEuxSbP4O14, x is trivalent europium ion Eu3+Substitute bismuth ion Bi3+Molar ratio, value range is
0.001≤x≤0.25。
The present invention also provides a kind of preparation method of the red Illuminant nanometer fluorescent powder of above-mentioned europium ion activation, including it is following
Step:
(1) according to Formula B i1-xEuxSbP4O14, the stoichiometric ratio of each corresponding element, weighs in 0.001≤x≤0.25
Bi containing bismuth ion3+Compound, Eu containing europium ion3+Compound, Sb containing antimony ion5+Or Sb3+Compound and contain phosphonium ion
P5+Compound, weighed raw material is dissolved separately in deionized water, nitric acid or hydrochloric acid and is diluted with deionized water, then
The complexing agent that 1.5~2.0 times of the reaction raw materials object molal quantity is added among each solution, respectively obtains the mixed liquor of each raw material；
The complexing agent is one of citric acid, oxalic acid；
(2) mixed liquor of step (1) each raw material is slowly mixed together, the stirring 1~5 under conditions of temperature is 50~100 DEG C
Hour, it stands, obtain fluffy presoma after drying；
(3) the presoma precalcining in air atmosphere for obtaining step (2), calcination temperature are 450~750 DEG C, calcining
Time is 1~10 hour；
(4) by after the obtained mixture natural cooling of step (3), ground and mixed is uniform, calcines in air atmosphere, forges
Burning temperature is 850~1100 DEG C, and calcination time is 1~15 hour, obtains a kind of red Illuminant nanometer fluorescent powder of europium ion activation.
In above scheme, the Bi containing bismuth ion3+Compound be basic bismuth carbonate (BiO)2CO3·0.5H2O, bismuth nitrate
Bi(NO3)3·5H2One of O；The Eu containing europium ion3+Compound be europium oxide Eu2O3, europium nitrate Eu (NO3)3·
6H2One of O；The Sb containing antimony ion5+Or Sb3+Compound be antimony pentoxide Sb2O5, antimony trichloride SbCl3In
It is a kind of；The P containing phosphonium ion5+Compound be phosphorus pentoxide P2O5, ammonium dihydrogen phosphate NH4H2PO4, diammonium hydrogen phosphate
(NH4)2HPO4One of.
Preferably, the calcination temperature of above-mentioned steps (4) is 900~1000 DEG C, and calcination time is 8~12 hours.
The present invention also provides above-mentioned europium ion activation red Illuminant nanometer fluorescent powder application, the fluorescent powder it is ultraviolet,
Under near ultraviolet excitation can emission peak be located at the feux rouges of 614 rans, it is sharp for can be applied to ultraviolet, black light
During the various illuminations to rise are shown and luminescence generated by light coloration adjusts, it can also mix with blue, green emitting phosphor, coating and be encapsulated
In outside InGaN diode, the LED of capable of emitting warm white is prepared.
Compared with the prior art, the advantages of the present invention are as follows:
(1) present invention has effective light absorption in ultraviolet, near ultraviolet region, in the excitation of near ultraviolet region
Under, can emission peak be located at the feux rouges of 614 rans, luminous chromaticity coordinate value is x=0.625-0.655, y=
The red of 0.345-0.375, coloration are pure；The near ultraviolet semiconductor chips such as excitation wavelength and InAlGaN, InGaAs are very
Match, coated in white light LEDs can be prepared on blue-light LED chip, can be used as the depth in multiple bases energy conservation fluorescent light source LED and WLED
Red component with modulated light source colour temperature and improves colour rendering index.It can be also used for by ultraviolet light and blue light activated other be various
In lighting apparatus.
(2) in this field, europium ion Eu is adulterated in matrix3+When, europium ion Eu3+4f energy level split in crystalline field
It splits, and there is extremely big dependence to crystalline field, the 4f energy level of division is influenced by crystalline field is very big, is generated different
, luminescent transition abundant；Europium ion Eu3+Ground state be5D0Energy level, excitation state have7F0-4Different energy level, in different crystal
Among5D0→7F2With different intensity, therefore luminous intensity and color are all influenced by different substrates, in addition europium ion
Eu3+4f energy level resonance efficiency it is extremely low, be difficult to find suitable matrix.The application is by europium ion Eu3+It is doped to
BiSbP4O14In, the red fluorescence powder of uniform granularity, better crystallinity degree is obtained, granule size is suitble to be coated in nanometer range
Outside LED diode；Matrix stablize it is corrosion-resistant, and emit feux rouges it is high-efficient, coloration is pure；Use process is environmentally friendly, in purple
The toxic gases such as sulfide will not be generated under UV radiation.
(3) preparation process of the present invention is simple, easily operated, not high to working condition and equipment requirement, and is not necessarily to indifferent gas
Body protection, reduces energy consumption, at low cost and favorable repeatability；Production process is discharged without waste gas and waste liquid, is a kind of environment friend
Good phosphor.
Detailed description of the invention
Fig. 1 is the X-ray powder diffraction pattern that 1 technical solution of embodiment prepares sample；
Fig. 2 is the scanning electron microscopy spectrum of the material sample of 1 technical solution of embodiment preparation；
Fig. 3 is the excitation spectrum that embodiment 1 prepares that sample obtains under the monitoring of 614 nano red lights；
Fig. 4 is the luminous map that embodiment 1 prepares that sample obtains under 395 nanometers of black light excitations；
Fig. 5 is the scanning electron microscopy spectrum of the material sample of 5 technical solution of embodiment preparation；
Fig. 6 is the excitation spectrum that embodiment 5 prepares that sample obtains under the monitoring of 614 nano red lights；
Fig. 7 is the luminous map that embodiment 5 prepares that sample obtains under 395 nanometers of black light excitations；
Specific embodiment
Technical solution of the present invention is further described with reference to the accompanying drawings and examples.
Embodiment 1:
According to chemical formula Bi0.85Eu0.15SbP4O14The stoichiometry score of middle bismuth ion, europium ion, antimony ion and phosphonium ion
Also known as take basic bismuth carbonate (BiO)2CO3·0.5H2O:1.1028 grams；Europium nitrate Eu (NO3)3·6H2O:0.3345 grams；Tri-chlorination
Antimony SbCl3: 1.1406 grams；Diammonium hydrogen phosphate (NH4)2HPO4: 2.64 grams.Weighed raw material basic bismuth carbonate is dissolved in dilute nitre
Acid；Weighed europium nitrate, antimony trichloride, diammonium hydrogen phosphate are dissolved separately in deionized water；Then basic bismuth carbonate solution it
0.2162 gram of citric acid is added among 1.2249 grams of citric acids of middle addition, europium nitrate solution, is added among antimony trichloride solution
5.7642 grams of citric acids are added among 1.4411 grams of citric acids, ammonium dibasic phosphate solution, are stirred respectively, are obtained clear solution；
Four kinds of solution are slowly mixed together, are stirred 1 hour under conditions of temperature is 100 DEG C, are obtained after standing, drying fluffy
Presoma；The precalcining in air atmosphere by the presoma, calcination temperature are 750 DEG C, and calcination time is 1 hour；It is acquired
Mixture it is cooling after grind uniformly, calcined in air atmosphere, calcination temperature is 1000 DEG C, and calcination time is 8 hours, is obtained
A kind of red Illuminant nanometer fluorescent powder of europium ion activation.
Referring to attached drawing 1, it is the X-ray powder diffraction pattern that 1 technical solution of the present embodiment prepares sample, XRD test knot
Fruit shows that prepared material is monophase materials, and not any other impurity thing mutually exists.
Referring to attached drawing 2, it is the scanning electron microscopy spectrum by the sample of technical solution of embodiment of the present invention preparation, as a result
It has been shown that, the material crystalline is functional, and partial size is at 100~200 nanometers.
Referring to attached drawing 3, it is the exciting light obtained under the monitoring of 615 nano red lights by the sample of the technology of the present invention preparation
Spectrum, it can be seen that luminous excitation source can be well matched near ultraviolet to blue light diode chip mainly at 395 nanometers
Excitation requires；
Referring to attached drawing 4, it is shone by what the sample of the technology of the present invention preparation obtained under 395 nanometers of black light excitations
Spectrogram, the red light wave band that the main center emission wavelength of the material is 614 nanometers.
Embodiment 2:
According to chemical formula Bi0.999Eu0.001SbP4O14Among bismuth ion, europium ion, antimony ion and phosphonium ion stoichiometry
Than weighing bismuth nitrate Bi (NO respectively3)3·5H2O:2.4231 grams；Europium oxide Eu2O3: 0.0009 gram；Antimony pentoxide Sb2O5:
0.8088 gram；Ammonium dihydrogen phosphate NH4H2PO4: 2.3 grams.By weighed raw material bismuth nitrate and ammonium dihydrogen phosphate be dissolved separately in from
Sub- water；Weighed europium oxide is dissolved in dust technology；Weighed antimony pentoxide is dissolved in hydrochloric acid under 60 DEG C of heating；Nitric acid
0.8995 gram of oxalic acid is added among bismuth solution, 0.0009 gram of oxalic acid is added among europium oxide solution, among antimony pentoxide solution
It adds 0.9004 gram of oxalic acid, add 3.6016 grams of oxalic acid among ammonium dihydrogen phosphate, stir respectively, obtain clear solution；
Above four kinds of solution is slowly mixed together, is stirred 5 hours under conditions of temperature is 50 DEG C, stands, obtained after drying
Fluffy presoma；The precalcining in air atmosphere by the presoma, calcination temperature are 450 DEG C, and calcination time is 10 hours；Institute
It grinds uniformly after obtained mixture is cooling, is calcined in air atmosphere, calcination temperature is 900 DEG C, and calcination time is 12 hours,
Obtain a kind of red Illuminant nanometer fluorescent powder of europium ion activation.
The main structural behaviour of sample, excitation spectrum and luminescent spectrum are similar to Example 1.
Embodiment 3:
According to chemical formula Bi0.99Eu0.01SbP4O14Among bismuth ion, europium ion, antimony ion and phosphonium ion stoichiometric ratio
Bismuth nitrate Bi (NO is weighed respectively3)3·5H2O:2.4012 grams；Europium nitrate Eu (NO3)3·6H2O:0.0223 grams；Antimony pentoxide
Sb2O5: 0.8088 gram；Phosphorus pentoxide P2O5: 1.42 grams.Weighed raw material bismuth nitrate, phosphorus pentoxide are dissolved separately in
Ionized water；Weighed europium nitrate is dissolved in dust technology；Weighed antimony pentoxide is dissolved in hydrochloric acid under 60 DEG C of heating；So
0.8023 gram of oxalic acid is added among the bismuth nitrate solution afterwards, adds 0.0081 gram of oxalic acid, antimony pentoxide among europium nitrate solution
0.8104 gram of oxalic acid is added among solution, adds 3.2414 grams of oxalic acid among phosphorus pentoxide solution, is stirred, is clarified respectively
Solution；
Above four kinds of solution is slowly mixed together, is stirred 3 hours under conditions of temperature is 70 DEG C, stands, obtained after drying
Fluffy presoma；The precalcining in air atmosphere by the presoma, calcination temperature are 700 DEG C, and calcination time is 5 hours；Institute
It grinds uniformly after obtained mixture is cooling, is calcined in air atmosphere, calcination temperature is 900 DEG C, and calcination time is 8 hours,
Obtain a kind of red Illuminant nanometer fluorescent powder of europium ion activation.
The main structural behaviour of sample, excitation spectrum and luminescent spectrum are similar to Example 1.
Embodiment 4:
According to chemical formula Bi0.988Eu0.012SbP4O14Among bismuth ion, europium ion, antimony ion and phosphonium ion stoichiometry
Than weighing bismuth nitrate Bi (NO respectively3)3·5H2O:2.3964 grams；Europium oxide Eu2O3: 0.0106 gram；Antimony pentoxide Sb2O5:
0.8088 gram；Phosphorus pentoxide P2O5: 1.42 grams.Weighed raw material bismuth nitrate, phosphorus pentoxide are dissolved separately in deionization
Water；Weighed europium oxide is dissolved in dust technology；Weighed antimony pentoxide is dissolved in hydrochloric acid under 60 DEG C of heating；Then exist
1.6304 grams of citric acids are added among bismuth nitrate solution, 0.0196 gram of citric acid, antimony pentoxide are added among europium oxide solution
1.6332 grams of citric acids are added among solution, add 6.5328 grams of citric acids among phosphorus pentoxide solution, are stirred, are obtained respectively
Clear solution；
Above four kinds of solution is slowly mixed together, is stirred 2 hours under conditions of temperature is 80 DEG C, stands, obtained after drying
Fluffy presoma；The precalcining in air atmosphere by the presoma, calcination temperature are 650 DEG C, and calcination time is 3 hours；Institute
It grinds uniformly after obtained mixture is cooling, is calcined in air atmosphere, calcination temperature is 1100 DEG C, and calcination time is 1 hour,
Obtain a kind of red Illuminant nanometer fluorescent powder of europium ion activation.
The main structural behaviour of sample, excitation spectrum and luminescent spectrum are similar to Example 1.
Embodiment 5:
According to chemical formula Bi0.982Eu0.018SbP4O14Among bismuth ion, europium ion, antimony ion and phosphonium ion stoichiometry
Than weighing basic bismuth carbonate (BiO) respectively2CO3·0.5H2O:1.2741 grams；Europium nitrate Eu (NO3)3·6H2O:0.0401 grams；Three
Antimony chloride SbCl3: 1.1401 grams；Ammonium dihydrogen phosphate NH4H2PO4: 2.3 grams.Weighed raw material basic bismuth carbonate is dissolved in dilute nitre
Weighed europium nitrate, antimony trichloride, ammonium dihydrogen phosphate are dissolved separately in deionized water by acid；Then among basic bismuth carbonate
1.7925 grams of citric acids are added, 0.0329 gram of citric acid is added among europium nitrate solution, is added among antimony trichloride solution
7.3013 grams of citric acids are added among 1.8253 grams of citric acids, ammonium dihydrogen phosphate, are decomposed stirring respectively, are obtained clear molten
Liquid；
Above four kinds of solution is slowly mixed together, is stirred 4 hours under the conditions of at a temperature of 90 °C, stands, obtained after drying
Fluffy presoma；The precalcining in air atmosphere by the presoma, calcination temperature are 550 DEG C, and calcination time is 6 hours；Institute
It grinds uniformly after obtained mixture is cooling, is calcined in air atmosphere, calcination temperature is 850 DEG C, and calcination time is 15 hours,
Obtain a kind of europium ion Eu3+The red Illuminant nanometer fluorescent powder of activation.The XRD diffraction pattern of the embodiment is as embodiment 1.
Referring to the scanning electron microscopy spectrum that attached drawing 5 is by the material sample of technical solution of embodiment of the present invention preparation, knot
Fruit shows that the material crystalline is functional, and partial size is at 100~200 nanometers.
Referring to attached drawing 6, from the excitation obtained under the monitoring of 614 nano red lights to the material sample prepared by the technology of the present invention
Spectrum, in figure as can be seen that luminous excitation source is mainly at 395 nanometers, therefore the excitation of the emitting red light of the material can be with
Match ultraviolet-near ultraviolet LED chip.
It is the luminescent spectrum figure that sample obtains under 395 nanometers of black light excitations referring to attached drawing 7, can be seen that in figure
The red light wave band that the main center emission wavelength of the material is 614 nanometers.
Embodiment 6:
According to chemical formula Bi0.979Eu0.021SbP4O14Among bismuth ion, europium ion, antimony ion and phosphonium ion stoichiometry
Than weighing basic bismuth carbonate (BiO) respectively2CO3·0.5H2O:1.2702 grams；Europium nitrate Eu (NO3)3·6H2O:0.0468 grams；Three
Antimony chloride SbCl3: 1.1401 grams；Ammonium dihydrogen phosphate NH4H2PO4: 2.3 grams.Weighed raw material basic bismuth carbonate is dissolved in dilute nitre
Weighed europium nitrate, antimony trichloride, ammonium dihydrogen phosphate are dissolved separately in deionized water by acid；Then in basic bismuth carbonate solution
Among add 0.8815 gram of oxalic acid, 0.0189 gram of oxalic acid added among europium nitrate solution, is added among antimony trichloride solution
3.6016 grams of oxalic acid are added among 0.9004 gram of oxalic acid, ammonium dihydrogen phosphate, are stirred respectively, are obtained clear solution；
Above four kinds of solution is slowly mixed together, is stirred 3 hours under conditions of temperature is 95 DEG C, stands, obtained after drying
Fluffy presoma；The precalcining in air atmosphere by the presoma, calcination temperature are 730 DEG C, and calcination time is 3 hours；Institute
It grinds uniformly after obtained mixture is cooling, is calcined in air atmosphere, calcination temperature is 930 DEG C, and calcination time is 6 hours,
Obtain a kind of red Illuminant nanometer fluorescent powder of europium ion activation.
The main structural behaviour of sample, excitation spectrum and luminescent spectrum are similar to Example 5.
Embodiment 7:
According to chemical formula Bi0.975Eu0.025SbP4O14Among bismuth ion, europium ion, antimony ion and phosphonium ion stoichiometry
Than weighing bismuth nitrate Bi (NO respectively3)3·5H2O:2.3649 grams；Europium nitrate Eu (NO3)3·6H2O:0.5576 grams；Antimony trichloride
SbCl3: 1.1406 grams；Ammonium dihydrogen phosphate NH4H2PO4: 2.3 grams.By weighed raw material bismuth nitrate, europium nitrate, antimony trichloride, phosphorus
Acid dihydride ammonium is dissolved separately in deionized water；Then 0.0183 gram of citric acid, europium nitrate solution are added among bismuth nitrate solution
Among add 0.0480 gram of citric acid, add 1.9214 grams of citric acids among antimony trichloride solution, among ammonium dihydrogen phosphate
7.6856 grams of citric acids are added, are stirred respectively, clear solution is obtained；
Above four kinds of solution is slowly mixed together, is stirred 2.5 hours under conditions of temperature is 85 DEG C, stands, obtained after drying
To fluffy presoma；The precalcining in air atmosphere by the presoma, calcination temperature are 680 DEG C, and calcination time is 5 hours；
It grinds uniformly after obtained mixture is cooling, is calcined in air atmosphere, calcination temperature is 930 DEG C, and calcination time is 5 small
When, obtain a kind of red Illuminant nanometer fluorescent powder of europium ion activation.
The main structural behaviour of sample, excitation spectrum and luminescent spectrum are similar to Example 5.
Claims (5)
1. a kind of nano-phosphor that glows of europium ion activation, it is characterised in that: chemical formula Bi1-x Eu x SbP4O14,xIt is three
Valence europium ion Eu3+Substitute bismuth ion Bi3+Molar ratio, value range be 0.001≤x≤0.25。
2. a kind of preparation method of the nano-phosphor that glows of europium ion activation as described in claim 1, which is characterized in that
The following steps are included:
(1) according to Formula B i1-x Eu x SbP4O14, 0.001≤xThe stoichiometric ratio of each corresponding element in≤0.25, weigh bismuth-containing from
Sub- Bi3+Compound, Eu containing europium ion3+Compound, Sb containing antimony ion5+Or Sb3+Compound and chemical combination containing phosphonium ion
Weighed raw material is dissolved separately in deionized water, nitric acid or hydrochloric acid and is diluted with deionized water by object, then in each solution
Among add the complexing agent of 1.5~2.0 times of the reaction raw materials object molal quantity, respectively obtain the mixed liquor of each raw material；The network
Mixture is one of citric acid, oxalic acid；
(2) mixed liquor of step (1) each raw material is slowly mixed together, is stirred 1~5 hour under conditions of temperature is 50~100 DEG C,
It stands, obtain fluffy presoma after drying；
(3) the presoma precalcining in air atmosphere for obtaining step (2), calcination temperature are 450~750 DEG C, calcination time
It is 1~10 hour；
(4) by after the obtained mixture natural cooling of step (3), ground and mixed is uniform, calcines in air atmosphere, calcining temperature
Degree is 850~1100 DEG C, and calcination time is 1~15 hour, obtains a kind of red Illuminant nanometer fluorescent powder of europium ion activation.
3. the preparation method of the nano-phosphor that glows of europium ion activation according to claim 2, it is characterised in that: institute
State Bi containing bismuth ion3+Compound be basic bismuth carbonate (BiO)2CO3•0.5H2O, bismuth nitrate Bi (NO3)3•5H2One of O；
The Eu containing europium ion3+Compound be europium oxide Eu2O3, europium nitrate Eu (NO3)3·6H2One of O；Described contains antimony
Ion Sb5+Or Sb3+Compound be antimony pentoxide Sb2O5, antimony trichloride SbCl3One of；It is described containing phosphonium ion
Compound is phosphorus pentoxide P2O5, ammonium dihydrogen phosphate NH4H2PO4, diammonium hydrogen phosphate (NH4)2 HPO4One of.
4. the preparation method of the nano-phosphor that glows of europium ion activation according to claim 2, it is characterised in that: step
Suddenly the calcination temperature of (4) is 900~1000 DEG C, and calcination time is 8~12 hours.
5. a kind of application of the nano-phosphor that glows of europium ion activation as described in claim 1, which is characterized in that this is glimmering
Light powder it is ultraviolet, under near ultraviolet excitation can emission peak be located at the feux rouges of 614 rans, can be applied to it is ultraviolet,
Black light is that during the various illuminations of excitaton source are shown and luminescence generated by light coloration adjusts, can also mix it with blue, green emitting phosphor
It closes, applies and be packaged in outside InGaN diode, prepare the LED of capable of emitting warm white.
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| CN115449370B (en) * | 2022-09-05 | 2023-08-04 | 江苏迪飞达电子有限公司 | Red luminous fluorescent powder with europium ion as activator and preparation method thereof |
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