CN106995698A - A kind of preparation method for launching enhanced fluorescent material - Google Patents
A kind of preparation method for launching enhanced fluorescent material Download PDFInfo
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- CN106995698A CN106995698A CN201710202316.2A CN201710202316A CN106995698A CN 106995698 A CN106995698 A CN 106995698A CN 201710202316 A CN201710202316 A CN 201710202316A CN 106995698 A CN106995698 A CN 106995698A
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- 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
- C09K11/7734—Aluminates
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Abstract
The use of metal simple-substance powder is reducing agent, metal simple-substance powder is Al, Ti or Mg, by Ca the invention provides a kind of preparation method for launching enhanced fluorescent material2SiO4:Eu presomas are contained in the first quartz glass tube, reducing agent and Ca2SiO4:The mass ratio of Eu powder is（0.05~1）: 1, then the first quartz glass tube is put in the second quartz glass tube that bottom fills metal simple-substance powder, using oxyhydrogen flame sealer by the second quartz glass tube sealed after being vacuumized, it is placed in Muffle furnace, under the conditions of 600 1000 DEG C, carry out heating 6 ~ 10h, produce the enhanced Ca of transmitting2SiO4:Eu fluorescent material.Ca prepared by the present invention2SiO4:Eu powder is that CO reducing agents prepare Ca2SiO4:2.8 times of Eu powder emissive porwers.
Description
Technical field
The invention belongs to chemical field, it is related to a kind of fluorescent material, specifically a kind of system for launching enhanced fluorescent material
Preparation Method.
Background technology
White light LEDs are a kind of New Solid lighting sources, compared with traditional incandescent lamp, fluorescent lamp, with small power consumption, effect
Rate height, environmental protection, energy-conservation, long lifespan, small volume, the remarkable advantage such as response is fast, colour rendering is good, it is environmentally friendly as new generation of green
Lighting source, with wide market prospects and huge economic results in society, has obtained the extensive concern of industry.At present, base
Mainly there are 3 kinds in the LED modes for producing white light emission：(1) polychromatic combination method, i.e., produced by red, green, blue three mixture of colours
Raw white light, such as combination red, green, blue (RGB) Tricolor LED；(2) RGB fluorescent material is excited using ultraviolet LED；(3) use
Blue LED excites yellow fluorescent powder.Wherein, the assembled scheme color developing of RGB fluorescent material is excited most with ultraviolet LED
It is good, but be due to insensitivity of the vision to ultraviolet-black light, the color of this kind of white light LEDs is only determined by fluorescent material, therefore
Research and development are particularly important available for the three primary colors fluorescent powder of near ultraviolet (350~420nm) type white light LEDs (NUV-LED).
Ca2SiO4:Eu2+Green emitting phosphor is because excitation wavelength range is wide, luminosity is high, good chemical stability, and by state
Inside and outside researcher is widely studied.As researcher passes through solid reaction process, sol-gel process, coprecipitation, liquid phase legal system
The method such as standby prepares the Ca of different-shape2SiO4:Eu2+.Also substantial amounts of research work passes through impurity or substituted side
Formula, to improve Ca2SiO4:Eu2+Spectrum.In Ca2SiO4:Eu2+Reduction preparation process in, method conventional at present is nitrogen hydrogen
Reducing process and carbothermy.Wherein carbothermic method mainly uses inorganic carbon dust in heating process because excessive in local environment
And produce CO method to be reduced.However, CO belongs to weak atmosphere reduction, in addition during the cladding of carbon dust, it is difficult to pair
Each reducing condition carries out quantitative setting, causes assay reproducibility poor.In addition, fluorescent material prepared by this method is often subject to
The pollution and influence of carbon dust are remained, directly results in and is affected.Nitrogen hydrogen reduction rule is mixed with a certain proportion of nitrogen/hydrogen
Gas, depends on H2Reduction come the method for realizing the preparation of fluorescent material.This method reduction effect is relatively preferable, does not have
The problems such as having Carbon dust pollution in carbothermic method, but there is also because of H simultaneously2Caused by leakage the problems such as security.Based on
On investigation, we yet there are no so far on using metal simple-substance powder be reducing agent prepare Ca2SiO4:Eu fluorescent material simultaneously changes
It is apt to the report of its spectral quality.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of preparation side for launching enhanced fluorescent material
Method, the preparation method of the described enhanced fluorescent material of this transmitting will solve Ca prepared by the method for prior art2SiO4:Eu is glimmering
The not high technical problem of the emissive porwer of light powder.
The invention provides the enhanced Ca of one kind transmitting2SiO4:Eu fluorescent material and preparation method thereof, uses metal simple-substance powder
End is reducing agent, and described metal simple-substance powder is Al, Ti or Mg, by Ca2SiO4:Eu presomas are contained in the first quartz glass
Guan Zhong, described reducing agent and Ca2SiO4:The mass ratio of Eu powder is (0.05~1): 1, then the first quartz glass tube is put in
Bottom is filled in the second quartz glass tube of metal simple-substance powder, and the diameter of described the second quartz glass tube is more than described the
The diameter of one quartz glass tube, using oxyhydrogen flame sealer by the second quartz glass tube sealed after being vacuumized, is placed in Muffle furnace
In, under the conditions of 600-1000 DEG C, carry out heating 6~10h, produce the enhanced Ca of transmitting2SiO4:Eu fluorescent material.
Further, 8h is heated in Muffle furnace.
Further, described reducing agent and Ca2SiO4:The mass ratio of Eu powder is 0.1: 1.
The present invention is reducing agent using metal simple-substance, by Ca2SiO4:Eu powder presomas are contained in the semiclosed quartzy glass of internal layer
In glass pipe, then it is put in the semiclosed quartz glass tube of outer layer that bottom fills metal simple-substance powder, uses oxyhydrogen flame sealer
By outer layer quartz glass tube sealed after being vacuumized, it is placed in being heated in Muffle furnace.By the present invention in that using metal list
Matter powder, by contactless reduction treatment, improves Ca as reducing agent2SiO4:Eu green emitting phosphor emissive porwers, from
And it is preferably applied for white light LED part.
The present invention is compared with prior art, and its technological progress is significant.The present invention is compared to H2Reducing process, present invention side
Method is safe and reliable；Compared to CO reducing process, the inventive method is environment friendly and pollution-free, and harmful gas such as CO will not be produced in course of reaction
Body；And the method Ca simple to operate, prepared of the present invention2SiO4:The spectral intensity of Eu fluorescent material is reduced higher than traditional CO
Ca prepared by method2SiO4:Eu fluorescent material.
Brief description of the drawings
Fig. 1 is Ca obtained by this method2SiO4:The fluorescent emission spectrogram of Eu powder, (380nm), this hair under near ultraviolet excitation
Ca prepared by bright method2SiO4:Eu prepares the Ca of (with the conditions of 1000 DEG C of processing 8h) with CO reducing process2SiO4:Eu is luminous strong
Degree compares.
Embodiment：
Embodiment 1
Ca2SiO4:Eu presomas are prepared by synthesis by solid state reaction：To prepare 3g Ca2SiO4:Exemplified by 0.005Eu, press
3.464g CaCO are accurately weighed according to stoichiometric proportion3, 1.0397g SiO2, 0.0152g Eu2O3, load weighted raw material is shifted
After being well mixed into agate mortar, be contained in crucible, be subsequently placed in Muffle furnace and under conditions of 1250 DEG C heating it is 8 small
When, it is cooled to after room temperature, takes out powder and produce Ca2SiO4:Eu presomas.
According to Al powder and Ca2SiO4:The mass ratio 0.1: 1 of Eu powder presomas weighs 0.3g Al powder and 3g Ca2SiO4:Eu
Powder presoma, by Ca2SiO4:Eu powder presomas are contained in a diameter of 8mm quartz glass tube, are then put in bottom and are filled gold
In the quartz glass tube for belonging to a diameter of 10mm of elemental powders, outer layer quartz glass tube is vacuumized using oxyhydrogen flame sealer rear close
Envelope, is placed in Muffle furnace being heated in 600 DEG C, 700 DEG C, 800 DEG C, 900 DEG C, 1000 DEG C, naturally cold after reduction 8h
But to room temperature, the target fluorescent powder Ca after taking-up processing2SiO4:Eu。
In whole preparation process, the diameter 8mm quartz glass tubes placed in Muffle furnace are semiclosed, diameter 10mm quartz glass
Glass pipe is totally-enclosed.
Test its luminous intensity using XRF (HITACHI F-7000), under the conditions of same test, by with
CO reducing process reduces 8h Ca at 1000 DEG C2SiO4:It (is all 380nm near ultraviolet excitations, 1000 that the luminous intensity of Eu powder, which compares,
DEG C processing 8h conditions), Ca prepared by the present invention2SiO4:Eu powder is that CO reducing agents prepare Ca2SiO4:The 2.8 of Eu powder emissive porwers
Times.(as shown in Figure 1).
The concrete case of table 1
Claims (3)
1. a kind of preparation method for launching enhanced fluorescent material, it is characterised in that：The use of metal simple-substance powder is reducing agent, it is described
Metal simple-substance powder be Al, Ti or Mg, by Ca2SiO4:Eu presomas are contained in the first quartz glass tube, described reduction
Agent and Ca2SiO4:The mass ratio of Eu powder is（0.05~1）: 1, the first quartz glass tube is then put in bottom and fills metal list
In second quartz glass tube of matter powder, the diameter of the second described quartz glass tube is more than the first described quartz glass tube
Diameter, using oxyhydrogen flame sealer by the second quartz glass tube sealed after being vacuumized, is placed in Muffle furnace, at 600-1000 DEG C
Under the conditions of, carry out heating 6 ~ 10h, produce the enhanced Ca of transmitting2SiO4:Eu fluorescent material.
2. a kind of preparation method for launching enhanced fluorescent material according to claim 1, it is characterised in that：In Muffle furnace
Heat 8h.
3. a kind of preparation method for launching enhanced fluorescent material according to claim 1, it is characterised in that：Described reduction
Agent and Ca2SiO4:The mass ratio of Eu powder is 0.1: 1.
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| CN201710202316.2A CN106995698A (en) | 2017-03-30 | 2017-03-30 | A kind of preparation method for launching enhanced fluorescent material |
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| CN201710202316.2A CN106995698A (en) | 2017-03-30 | 2017-03-30 | A kind of preparation method for launching enhanced fluorescent material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609128A (en) * | 2018-12-29 | 2019-04-12 | 上海应用技术大学 | A kind of green emitting phosphor and preparation method thereof |
| CN109628084A (en) * | 2018-12-29 | 2019-04-16 | 上海应用技术大学 | A kind of blue colour fluorescent powder and its fast preparation method |
| CN109679654A (en) * | 2018-12-29 | 2019-04-26 | 上海应用技术大学 | A kind of fluorescent powder and preparation method thereof |
| CN110283592A (en) * | 2019-07-11 | 2019-09-27 | 上海应用技术大学 | A kind of CaO-SiO2- EuO full spectrum fluorescent powder and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104388081A (en) * | 2014-09-28 | 2015-03-04 | 东北大学 | Synthetic method for aluminate doped with valence-state-controllable rare earth element and product thereof |
| CN105038787A (en) * | 2015-07-01 | 2015-11-11 | 上海应用技术学院 | Ce, Tb and Mn-coactivated single-matrix phosphate white phosphor powder and preparation method thereof |
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2017
- 2017-03-30 CN CN201710202316.2A patent/CN106995698A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104388081A (en) * | 2014-09-28 | 2015-03-04 | 东北大学 | Synthetic method for aluminate doped with valence-state-controllable rare earth element and product thereof |
| CN105038787A (en) * | 2015-07-01 | 2015-11-11 | 上海应用技术学院 | Ce, Tb and Mn-coactivated single-matrix phosphate white phosphor powder and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| JONG SU KIM: "Temperature-dependent emission spectra of M2SiO4:Eu2+(M=Ca、Sr、Ba) phosphors for green and greenish white LEDs", 《SOLID STATE COMMUNICATIONS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609128A (en) * | 2018-12-29 | 2019-04-12 | 上海应用技术大学 | A kind of green emitting phosphor and preparation method thereof |
| CN109628084A (en) * | 2018-12-29 | 2019-04-16 | 上海应用技术大学 | A kind of blue colour fluorescent powder and its fast preparation method |
| CN109679654A (en) * | 2018-12-29 | 2019-04-26 | 上海应用技术大学 | A kind of fluorescent powder and preparation method thereof |
| CN110283592A (en) * | 2019-07-11 | 2019-09-27 | 上海应用技术大学 | A kind of CaO-SiO2- EuO full spectrum fluorescent powder and preparation method thereof |
| WO2021004224A1 (en) * | 2019-07-11 | 2021-01-14 | 上海应用技术大学 | Cao-sio2-euo full spectrum fluorescent powder and preparation method therefor |
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Application publication date: 20170801 |