CN105419798B - A kind of preparation method and application of orange red antimonate luminescent materials - Google Patents
A kind of preparation method and application of orange red antimonate luminescent materials Download PDFInfo
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Abstract
The invention discloses a kind of preparation method and application of orange red antimonate luminescent materials, belong to phosphor field.Its chemical general formula is Ca5‑5xEu5xSb5O17, wherein x is Eu3+The mole percent of doping, 0.001≤x≤0.15；Of the invention main using high temperature solid-state method and chemical synthesis, the orange red fluorescent powder prepared can be excited by light of the wavelength in 200~450 nanometer ranges, launch orange light of the dominant wavelength at 612 nanometers.The present invention is raw materials used cheap and easy to get, and preparation technology is simple, it is easy to operate, and the chemical property of matrix is stable, has excellent luminescent properties, is had broad application prospects in field of LED illumination.
Description
Technical field
The present invention relates to a kind of preparation method and application of orange red antimonate luminescent materials, more particularly to a kind of wavelength exists
The preparation method of the orange red stibate phosphor material powder of ultraviolet, near ultraviolet and excited by visible light in 200 ~ 450 nanometer ranges
And its application.
Background technology
Since the new century, the energy how is saved and environmental protection is always major issue that people are faced, in hair
Optical arena, white light LEDs have more preferable energy-saving effect, and stable luminescent property relative to traditional incandescent lamp, and service life is long,
So as to greatly reduce the loss to the energy, the green energy resource of new century is described as by people, and cause the widely studied of people.
Current most popular white light LEDs are mainly with GaN base chip collocation YAG：Ce fluorescent material, by exciting
YAG：What Ce realized to launch gold-tinted with blue light.But due to lacking red color light component in its light source, cause its colour developing to refer to
Number is than relatively low, and color reducibility is poor, the colder tone of tone so that in numerous lamp red fluorescence powders, really can practicality
And it is few, therefore the red fluorescence powder with efficient absorption turns into and studied both at home and abroad at present in the near ultraviolet to blue light range
Focus.
Stibate is widely used in fluorescent material with its abundant species and stable physicochemical properties by people
Host material, this has good optical absorption band mainly due to stibate, and the light through high-energy can be by absorption after exciting
Energy transmission gives the rare earth ion being entrained in metaantimmonic acid salt matrix, so as to reach luminous effect.Adulterated in metaantimmonic acid base status
Europium ion Eu3+The red fluorescence powder prepared has good colouring intensity and pure colourity, and this point is in Xin Lin et al.
The Ca of the structure of double perovskite of report2LaSbO6：There is good introduction in Eu red fluorescence powders.We grind on the basis of reporting herein
Study carefully the orange red luminescent material of calcium antimonate, and this phosphor material powder was not yet reported at present.
The content of the invention
It is an object of the invention to overcome the shortcomings of existing lamp phosphor technology, there is provided a kind of preparation technology is simple, property
Can the metaantimmonic acid alkali orange red fluorescent powder material that be able to can be adjusted between 550 ~ 650 of efficient and emission peak, make it in purple
Under outer and the exciting of visible ray, launch the orange light of efficient stable.
To achieve the above object, the technical solution adopted by the present invention is：A kind of orange red antimonate luminescent materials are provided, it
Chemical general formula be Ca5-5xEu5xSb5O17, wherein x is Eu3+The mole percent of doping, 0.001≤x≤0.15；Described antimony
Hydrochlorate based luminescent material has very strong response to the light in 200~450 nanometer ranges, can launch dominant wavelength and be received 612
The orange light of rice.
A kind of preparation method of orange red antimonate luminescent materials, using high temperature solid-state method, it is characterised in that including as follows
Step：
（1）By chemical formula Ca5-5xEu5xSb5O17The stoichiometric proportion of middle each element, wherein 0.001≤x≤0.15, respectively
Weigh containing calcium ion Ca2+Compound, contain europium ion Eu3+Compound, contain antimony ion Sb3+Compound, grinding simultaneously
It is well mixed, obtain mixture；
（2）By step（1）Obtained mixture is placed in Muffle furnace, in air atmosphere precalcining, and precalcining temperature is
300~700 DEG C, precalcination time is 2~16 hours；
（3）By step（2）Obtained mixture natural cooling, after grinding and being well mixed, is again placed in Muffle furnace,
Calcined in air atmosphere, calcining heat is 700~1100 DEG C, and calcination time is 1~12 hour, naturally cools to room temperature, is ground
Obtain a kind of to launch the stibate luminescent material of orange light under ultraviolet, near ultraviolet excitation after uniform.
Further, step（2）Precalcining temperature be 350~650 DEG C, precalcination time be 3~12 hours.
Further, step（3）Calcining heat be 750~1000 DEG C, calcination time be 2~9 hours.
Further, calcium ions Ca2+Compound be calcium carbonate, calcium chloride, calcium nitrate, calcium hydroxide, calcium oxide in
One kind；Described contains europium ion Eu3+Compound be europium oxide, europium nitrate, Europium chloride in one kind；Described contains antimony
Ion Sb3+Compound be antimony oxide, antimony chloride or nitric acid antimony in one kind.
A kind of preparation method of orange red antimonate luminescent materials, using chemical synthesis, comprises the following steps：
（1）By chemical formula Ca5-5xEu5xSb5O17The stoichiometric proportion of middle each element, wherein 0.001≤x≤0.15, respectively
Weigh containing calcium ion Ca2+Compound, contain europium ion Eu3+Compound, contain antimony ion Sb3+Compound, by them
Dust technology and deionized water dissolving are used respectively, then add complexing agent citric acid respectively by 0.5 ~ 2.0wt% of each reactant quality
Or oxalic acid, obtain the mixed solution of each raw material；
（2）By step（1）Obtained each mixed solution is slowly mixed together uniformly, is then stirred under 50~80 DEG C of temperature conditionss
Mix 1~2 hour, bulk presoma is obtained after standing, drying；
（3）By step（2）Obtained presoma is placed in Muffle furnace and calcined, and calcining heat is 500~950 DEG C, during calcining
Between be 2~10 hours, naturally cool to room temperature, obtaining one kind after grinding is uniform can launch under ultraviolet, near ultraviolet excitation
The stibate luminescent material of orange light.
Further, step（3）Calcining heat be 600~900 DEG C, calcination time be 3~9 hours.
Further, described calcium ions Ca2+Compound be calcium carbonate, calcium chloride, calcium nitrate, calcium hydroxide, oxygen
Change one kind in calcium；Described contains europium ion Eu3+Compound be europium oxide, europium nitrate, Europium chloride in one kind；Described
Contain antimony ion Sb3+Compound be antimony oxide, antimony chloride or nitric acid antimony in one kind.A kind of orange red stibate fluorescence
Regulation of the materials application in various luminous lighting materials with luminescence generated by light colourity.
Compared with prior art, the invention has the advantages that：The stibate base fluorescent powder that the present invention is provided has abundant
Species, with wider absorption band and higher translucency, and relative to other fluorescent material, such as sulfide, halide is
The material of base, its environmental-protecting performance is more preferable.The stibate base fluorescent powder that the present invention is provided, the process of preparation is simple to operation, weight
Renaturation is good, and reducing atmosphere protection is not required in whole process, therefore reduces energy consumption, and for the less demanding of equipment,
Greatly reduce the cost of production.Stibate base fluorescent powder designed by the present invention, can be by wavelength in 200~450 nanometers of models
Light in enclosing is excited, and is launched the orange light of 550-650 nanometer ranges, be can apply in new white light LEDs.
Brief description of the drawings
Fig. 1 is that the embodiment of the present invention 1 prepares sample Ca4.95Eu0.05Sb5O17X-ray powder diffraction pattern.
Fig. 2 is that the embodiment of the present invention 1 prepares sample Ca4.95Eu0.05Sb5O17SEM（SEM）Collection of illustrative plates.
Fig. 3 is that the embodiment of the present invention 1 prepares sample Ca4.95Eu0.05Sb5O17Excitation spectrum under the monitoring of 612 nano wave lengths
Figure.
Fig. 4 is that the embodiment of the present invention 1 prepares sample Ca4.95Eu0.05Sb5O17Luminescent spectrum in the case where 396 nano wave lengths are excited
Figure.
Fig. 5 is that the embodiment of the present invention 1 prepares sample Ca4.95Eu0.05Sb5O17Decay of luminescence under the monitoring of 612 nano wave lengths
Curve.
Fig. 6 is that the embodiment of the present invention 5 prepares sample Ca4.25Eu0.75Sb5O17X-ray powder diffraction pattern.
Fig. 7 is that the embodiment of the present invention 5 prepares sample Ca4.25Eu0.75Sb5O17SEM（SEM）Collection of illustrative plates.
Fig. 8 is that the embodiment of the present invention 5 prepares sample Ca4.25Eu0.75Sb5O17Excitation spectrum under the monitoring of 612 nano wave lengths
Figure.
Fig. 9 is that the embodiment of the present invention 5 prepares sample Ca4.25Eu0.75Sb5O17Luminescent spectrum in the case where 396 nano wave lengths are excited
Figure.
Figure 10 is that the embodiment of the present invention 5 prepares sample Ca4.25Eu0.75Sb5O17Luminous declining under the monitoring of 612 nano wave lengths
Subtract curve.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1：
Prepare Ca4.95Eu0.05Sb5O17
According to chemical formula Ca4.95Eu0.05Sb5O17The stoichiometric proportion of middle each element, weighs calcium carbonate CaCO respectively3：
0.9900 gram, europium oxide Eu2O3：0.0352 gram, antimony oxide Sb2O3：1.4575 grams, grind and mix in agate mortar
After uniform, air atmosphere precalcining 3 hours at 650 DEG C in Muffle furnace are selected, are then cooled to room temperature, sample is taken out；Again
Compound is sufficiently mixed grinding uniformly, among air atmosphere, is calcined 2 hours at 1000 DEG C, is cooled to room temperature, after taking-up simultaneously
It is fully ground and obtains powdered to launch the metaantimmonic acid salt material of orange light.
Referring to accompanying drawing 1, it is the X-ray powder diffraction pattern that the present embodiment technical scheme prepares sample, XRD test results
Occur in display, figure without other miscellaneous peaks, illustrate that obtained sample is single-phase material；
Referring to accompanying drawing 2, it is the SEM of the sample as prepared by the present embodiment technical scheme（SEM）Collection of illustrative plates；
It can be seen that gained sample crystallization is good, particle is uniformly dispersed, and its average grain diameter is 3.02 microns；
Referring to accompanying drawing 3, it is exciting light of the sample prepared by the present embodiment technical scheme under the monitoring of 612 nano wave lengths
Spectrogram；As seen from the figure, the material can well be excited by light of the wavelength in 200~450 nanometer ranges；
Referring to accompanying drawing 4, it is luminous light of the sample prepared by the present embodiment technical scheme in the case where 396 nano wave lengths are excited
Spectrogram, as seen from the figure, the material can launch orange light of the dominant wavelength in 612 nms；
Referring to accompanying drawing 5, it is that luminous under the monitoring of 612 nano wave lengths of the sample prepared by the present embodiment technical scheme declines
Subtract curve, can be calculated die-away time for 2.39 milliseconds.
Embodiment 2：
Prepare Ca4.9Eu0.1Sb5O17
According to chemical formula Ca4.9Eu0.1Sb5O17The stoichiometric proportion of middle each element, weighs calcium nitrate Ca (NO respectively3)2·
4H2O：2.3143 gram, europium oxide Eu2O3：0.0704 gram, antimony oxide Sb2O3：1.4575 grams, ground simultaneously in agate mortar
After well mixed, air atmosphere precalcining 8 hours at 450 DEG C in Muffle furnace are selected, are then cooled to room temperature, sample is taken out；
Compound is sufficiently mixed grinding uniformly again, among air atmosphere, is calcined 6 hours at 850 DEG C, is cooled to room temperature, taken out
Afterwards and it is fully ground and obtains powdered to launch the metaantimmonic acid salt material of orange light.
Its primary structure pattern, excitation spectrum, emission spectrum and attenuation curve are similar to Example 1.
Embodiment 3：
Prepare Ca4.85Eu0.15Sb5O17
According to chemical formula Ca4.85Eu0.15Sb5O17The stoichiometric proportion of middle each element, weighs calcium oxide CaO respectively：0.5439
Gram, Europium chloride EuCl3·6H2O：0.1099 gram, antimony oxide Sb2O3：1.4575 grams, grind and mix in agate mortar
After uniform, air atmosphere precalcining 6 hours at 550 DEG C in Muffle furnace are selected, are then cooled to room temperature, sample is taken out；Again
Compound is sufficiently mixed grinding uniformly, among air atmosphere, is calcined 4 hours at 950 DEG C, is cooled to room temperature, after taking-up simultaneously
It is fully ground and obtains powdered to launch the metaantimmonic acid salt material of orange light；
Its primary structure pattern, excitation spectrum, emission spectrum and attenuation curve are similar to Example 1.
Embodiment 4：
Prepare Ca4.8Eu0.2Sb5O17
According to chemical formula Ca4.8Eu0.2Sb5O17The stoichiometric proportion of middle each element, weighs calcium hydroxide Ca (OH) respectively2：
0.7113 gram, europium nitrate Eu (NO3)3·6H2O：0.1352 gram, antimony oxide Sb2O3：1.4575 grams, ground in agate mortar
After grinding and being well mixed, air atmosphere precalcining 12 hours at 350 DEG C in Muffle furnace are selected, are then cooled to room temperature, taken out
Sample；Compound is sufficiently mixed grinding uniformly again, among air atmosphere, is calcined 9 hours at 750 DEG C, is cooled to room temperature,
After taking-up and it is fully ground and obtains powdered to launch the metaantimmonic acid salt material of orange light；
Its primary structure pattern, excitation spectrum, emission spectrum and attenuation curve are similar to Example 1.
Embodiment 5：
Prepare Ca4.25Eu0.75Sb5O17
According to chemical formula Ca4.25Eu0.75Sb5O17The stoichiometric proportion of middle each element, weighs calcium chloride CaCl respectively2：
0.9433 gram, Europium chloride EuCl3·6H2O：0.5496 gram, antimony chloride SbCl3：2.8811 grams, and each raw material gross mass above
2.0wt% citric acid；Respectively above-mentioned raw materials, uniform stirring, until completely molten are dissolved with appropriate deionized water and nitric acid
Solution, is then complexed with citric acid, is finally uniformly mixed the good solution of above-mentioned complexing, be heated to 80 DEG C and stir respectively again
2 hours, stand, drying obtains bulk presoma；Precursor is placed in Muffle furnace and calcined, calcining heat is 900 DEG C, calcining
Time is 3 hours, is cooled to room temperature, after taking-up and is fully ground and obtains powdered to launch the stibate material of orange light
Material.
Referring to accompanying drawing 6, it is the X-ray powder diffraction pattern that the present embodiment technical scheme prepares sample, XRD test results
Occur in display, figure without other miscellaneous peaks, illustrate that obtained sample is single-phase material；
Referring to accompanying drawing 7, it is the SEM of the sample as prepared by the present embodiment technical scheme（SEM）Collection of illustrative plates；
It can be seen that gained sample particle is uniformly dispersed, its average grain diameter is 2.43 microns；
Referring to accompanying drawing 8, it is exciting light of the sample prepared by the present embodiment technical scheme under the monitoring of 612 nano wave lengths
Spectrogram；As seen from the figure, the material can well be excited by light of the wavelength in 200~450 nanometer ranges；
Referring to accompanying drawing 9, it is luminous light of the sample prepared by the present embodiment technical scheme in the case where 396 nano wave lengths are excited
Spectrogram, as seen from the figure, the material can launch orange light of the dominant wavelength in 612 nms；
Referring to accompanying drawing 10, it is that the sample prepared by the present embodiment technical scheme is luminous under the monitoring of 612 nano wave lengths
Attenuation curve, can be calculated die-away time for 3.23 milliseconds.
Embodiment 6：
Prepare Ca4.5Eu0.5Sb5O17
According to chemical formula Ca4.5Eu0.5Sb5O17The stoichiometric proportion of middle each element, weighs calcium nitrate Ca (NO respectively3)2·
4H2O：2.1253 gram, Europium chloride EuCl3·6H2O：0.3664 gram, antimony chloride SbCl3：2.8811 grams, and each raw material is total above
The 2.0wt% of quality citric acid；Respectively above-mentioned raw materials, uniform stirring, until completely are dissolved with appropriate deionized water and nitric acid
Dissolving, is then being complexed with citric acid, is finally uniformly being mixed the good solution of above-mentioned complexing, be heated to 80 DEG C and stir respectively
Mix 2 hours, stand, drying obtains bulk presoma；Precursor is placed in Muffle furnace and calcined, calcining heat is 800 DEG C, is forged
The burning time is 5 hours, is cooled to room temperature, after taking-up and is fully ground and obtains powdered to launch the stibate of orange light
Material.
Its primary structure pattern, excitation spectrum, emission spectrum and attenuation curve are similar to Example 5.
Embodiment 7：
Prepare Ca4.995Eu0.005Sb5O17
According to chemical formula Ca4.995Eu0.005Sb5O17The stoichiometric proportion of middle each element, weighs calcium chloride CaCl respectively2：
1.1087 grams, europium nitrate Eu (NO3)3·6H2O：0.0033 gram, nitric acid antimony Sb (NO3)3：2.1172 grams, and each raw material is total above
The 2.0wt% of quality citric acid；Respectively above-mentioned raw materials, uniform stirring, until completely are dissolved with appropriate deionized water and nitric acid
Dissolving, is then being complexed with citric acid, is finally uniformly being mixed the good solution of above-mentioned complexing, be heated to 80 DEG C and stir respectively
Mix 2 hours, stand, drying obtains bulk presoma；Precursor is placed in Muffle furnace and calcined, calcining heat is 700 DEG C, is forged
The burning time is 7 hours, is cooled to room temperature, after taking-up and is fully ground and obtains powdered to launch the stibate of orange light
Material.
Its primary structure pattern, excitation spectrum, emission spectrum and attenuation curve are similar to Example 5.
Embodiment 8
Prepare Ca4.975Eu0.025Sb5O17
According to chemical formula Ca4.975Eu0.025Sb5O17The stoichiometric proportion of middle each element, weighs calcium nitrate Ca respectively
(NO3)2·4H2O：2.3497 grams, europium nitrate Eu (NO3)3·6H2O：0.0169 gram, nitric acid antimony Sb (NO3)3：2.1172 gram, and
The 2.0wt% of each raw material gross mass of above citric acid；Above-mentioned raw materials are dissolved with appropriate deionized water and nitric acid respectively, uniformly
Stirring, until being completely dissolved, is then being complexed with citric acid, is finally uniformly being mixed the good solution of above-mentioned complexing respectively,
It is heated to 80 DEG C and stirs 2 hours, stands, drying obtains bulk presoma；Precursor is placed in Muffle furnace and calcined, calcining
Temperature is 600 DEG C, and calcination time is 9 hours, is cooled to room temperature, after taking-up and is fully ground and obtains powdered to launch
The metaantimmonic acid salt material of orange light.
Its primary structure pattern, excitation spectrum, emission spectrum and attenuation curve are similar to Example 5.
Claims (9)
1. a kind of orange red antimonate luminescent materials, it is characterised in that：Its chemical general formula is Ca5-5xEu5xSb5O17, wherein x is
Eu3+The mole percent of doping, 0.001≤x≤0.15.
2. a kind of preparation method of orange red antimonate luminescent materials, using high temperature solid-state method, it is characterised in that including following step
Suddenly：
（1）By chemical formula Ca5-5xEu5xSb5O17The stoichiometric proportion of middle each element, wherein 0.001≤x≤0.15, is weighed respectively
Contain calcium ion Ca2+Compound, contain europium ion Eu3+Compound, contain antimony ion Sb3+Compound, grind and mix
Uniformly, mixture is obtained；
（2）By step（1）Obtained mixture is placed in Muffle furnace, in air atmosphere precalcining, precalcining temperature be 300~
700 DEG C, precalcination time is 2~16 hours；
（3）By step（2）Obtained mixture natural cooling, after grinding and being well mixed, is again placed in Muffle furnace, in air
Calcined in atmosphere, calcining heat is 700~1100 DEG C, and calcination time is 1~12 hour, naturally cool to room temperature, grinding is uniform
Obtain a kind of to launch the stibate luminescent material of orange light under ultraviolet, near ultraviolet excitation afterwards.
3. a kind of a kind of preparation method of orange red antimonate luminescent materials as claimed in claim 2, it is characterised in that：Step
（2）Precalcining temperature be 350~650 DEG C, precalcination time be 3~12 hours.
4. a kind of a kind of preparation method of orange red antimonate luminescent materials as claimed in claim 2, it is characterised in that：Step
（3）Calcining heat be 750~1000 DEG C, calcination time be 2~9 hours.
5. a kind of a kind of preparation method of orange red antimonate luminescent materials as claimed in claim 2, it is characterised in that：It is described
Calcium ions Ca2+Compound be calcium carbonate, calcium chloride, calcium nitrate, calcium hydroxide, calcium oxide in one kind；Described contains
There is europium ion Eu3+Compound be europium oxide, europium nitrate, Europium chloride in one kind；Described contains antimony ion Sb3+Chemical combination
Thing is one kind in antimony oxide, antimony chloride or nitric acid antimony.
6. a kind of a kind of preparation method of orange red antimonate luminescent materials as claimed in claim 1, using chemical synthesis,
It is characterized in that comprising the following steps：
（1）By chemical formula Ca5-5xEu5xSb5O17The stoichiometric proportion of middle each element, wherein 0.001≤x≤0.15, is weighed respectively
Contain calcium ion Ca2+Compound, contain europium ion Eu3+Compound, contain antimony ion Sb3+Compound, they are distinguished
Complexing agent citric acid or grass are added respectively with dust technology and deionized water dissolving, then by 0.5 ~ 2.0wt% of each reactant quality
Acid, obtains the mixed solution of each raw material；
（2）By step（1）Obtained each mixed solution is slowly mixed together uniformly, then stirs 1 under 50~80 DEG C of temperature conditionss
~2 hours, bulk presoma is obtained after standing, drying；
（3）By step（2）Obtained presoma is placed in Muffle furnace and calcined, and calcining heat is 500~950 DEG C, and calcination time is 2
~10 hours, room temperature is naturally cooled to, orange light can be launched under ultraviolet, near ultraviolet excitation by obtaining one kind after grinding is uniform
Stibate luminescent material.
7. a kind of preparation method of orange red antimonate luminescent materials according to claim 6, it is characterised in that：Step
（3）Calcining heat be 600~900 DEG C, calcination time be 3~9 hours.
8. a kind of preparation method of orange red antimonate luminescent materials according to claim 6, it is characterised in that：Described
Calcium ions Ca2+Compound be calcium carbonate, calcium chloride, calcium nitrate, calcium hydroxide, calcium oxide in one kind；Described contains
Europium ion Eu3+Compound be europium oxide, europium nitrate, Europium chloride in one kind；Described contains antimony ion Sb3+Compound
For one kind in antimony oxide, antimony chloride or nitric acid antimony.
9. a kind of orange red antimonate luminescent materials as described in claim 1, it is characterised in that：Applied to luminous lighting material
Material neutralizes the regulation of luminescence generated by light colourity.
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| CN103232847A (en) * | 2013-01-23 | 2013-08-07 | 苏州大学 | Antimonite red phosphor powder for LED and preparation method thereof |
| CN103396796B (en) * | 2013-07-30 | 2015-03-25 | 苏州大学 | Antimonate long-afterglow fluorescent powder and preparation method thereof |
| CN103627392B (en) * | 2013-11-19 | 2015-12-02 | 苏州大学 | A kind of stibnate base red fluorescent powder and its preparation method and application |
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