CN105925263A - Calcium-titanium pyrophosphate fluorescent powder for LED and preparation method for calcium-titanium pyrophosphate fluorescent powder - Google Patents
Calcium-titanium pyrophosphate fluorescent powder for LED and preparation method for calcium-titanium pyrophosphate fluorescent powder Download PDFInfo
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- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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Abstract
The invention discloses calcium-titanium pyrophosphate fluorescent powder for an LED (Light-Emitting Diode) and a preparation method for the calcium-titanium pyrophosphate fluorescent powder. The composition of the calcium-titanium pyrophosphate fluorescent powder is Ca2-xTi(P2O7)2:xEu<2+>, wherein the value of the x is between 0.04 and 0.20; the calcium-titanium pyrophosphate fluorescent powder is prepared by the following steps: S1, weighing raw materials, namely, calcium carbonate, titanium dioxide and a mixture of sodium pyrophosphate and europium oxide according to the stoichiometric ratio of the Ca2-xTi(P2O7)2:xEu<2+>, wherein the value of the x is between 0.04 and 0.20; S2, adding a fluxing agent for grinding, and grinding uniformly to obtain a mixture; S3, putting the mixture obtained in the S2 into a crucible, sintering for 4 to 6 hours in a high-temperature furnace under the conditions of reducing atmosphere and 1,400 to 1,600 DEG C, and cooling to obtain the calcium-titanium pyrophosphate fluorescent powder, wherein the adding amount of the fluxing agent is 0.7 to 0.9 percent of the weight of the raw materials; the fluxing agent is a mixture of ammonium hydrogen phosphate and sodium nitrite; the ammonium hydrogen phosphate and the sodium nitrite are in the weight ratio of (6 to 8):1. The calcium-titanium pyrophosphate fluorescent powder provided by the invention has the advantages of high light intensity and high stability which are related to the weight ratio of the ammonium hydrogen phosphate to the sodium nitrite in the fluxing agent; the light intensity is highest when the ammonium hydrogen phosphate and the sodium nitrite are in the weight ratio of (6 to 8):1.
Description
Technical field
The invention belongs to field of light emitting materials, be specifically related to a kind of LED calcium pyrophosphate titanium fluorescent material and preparation method thereof.
Background technology
1974, first Holland succeeded in developing Philip the fluorescent material of red, green, blue three coloured light by sending human eye sensitivity
Yittrium oxide (glowing, peak wavelength is 611nm), many magnesium aluminates (green light, peak wavelength is 541nm) and many magnesium aluminates
(complete name is rare earth element three to barium (blue light-emitting, peak wavelength is 450nm) to be mixed into three primary colors fluorescent powder by a certain percentage
Primary colours fluorescent material), its luminous efficiency is high (average light efficiency is at 5 times of more than 80lm/W, about incandescent lamp), and colour temperature is
2500K-6500K, colour rendering index is about 85, and the raw material making fluorescent lamp with it can be greatly saved the energy, here it is energy-efficient
The cause of fluorescent lamp.It can be said that the exploitation of rare earth element three primary colors fluorescent powder is that in fluorescent lamp development history is important with application
Milestone.There is no three primary colors fluorescent powder, it is then not possible to have today of slim pipe diameter compact high efficiency energy saving fluorescent lamp of new generation.But it is dilute
Earth elements three primary colors fluorescent powder also has its shortcoming, and its disadvantage is exactly expensive.
Summary of the invention
It is an object of the invention to provide a kind of LED calcium pyrophosphate titanium fluorescent material and preparation method thereof.
The above-mentioned purpose of the present invention is achieved by techniques below scheme:
A kind of LED calcium pyrophosphate titanium fluorescent material, its chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein, x value
0.04～0.20, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.04～0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in reducing atmosphere and 1400～1600 DEG C of conditions in high temperature furnace
Lower sintering 4～6 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.7～0.9% of raw material weight, and described flux is the mixed of ammonium hydrogen phosphate and natrium nitrosum
The weight ratio of compound, ammonium hydrogen phosphate and natrium nitrosum is 6～8:1.
Further, described LED calcium pyrophosphate titanium fluorescent material, its chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein,
X value 0.10, is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 7:1.
Further, described LED calcium pyrophosphate titanium fluorescent material, its chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein,
X value 0.04, is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.04；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1400 DEG C
Tie 6 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 6:1.
Further, described LED calcium pyrophosphate titanium fluorescent material, its chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein,
X value 0.20, is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1600 DEG C
Tie 4 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 8:1.
Further, described reducing atmosphere is Carbon monoxide reduction atmosphere.
Advantages of the present invention:
The calcium pyrophosphate titanium light-emitting phosphor intensity that the present invention provides is high, and stability is high, these advantages and ammonium hydrogen phosphate in flux
Relevant with the weight ratio of natrium nitrosum, when the weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 6～8:1, luminous intensity is the highest.
Detailed description of the invention
Further illustrate the essentiality content of the present invention below in conjunction with embodiment, but do not limit scope with this.To the greatest extent
The present invention is explained in detail by pipe with reference to preferred embodiment, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent, without deviating from the spirit and scope of technical solution of the present invention.
Embodiment 1: the preparation of calcium pyrophosphate titanium fluorescent material
Chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 7:1.
Embodiment 2: the preparation of calcium pyrophosphate titanium fluorescent material
Chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein, x value 0.04, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.04；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1400 DEG C
Tie 6 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 6:1.
Embodiment 3: the preparation of calcium pyrophosphate titanium fluorescent material
Chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein, x value 0.20, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1600 DEG C
Tie 4 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 8:1.
Embodiment 4: the preparation of calcium pyrophosphate titanium fluorescent material
Chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 6:1.
Embodiment 5: the preparation of calcium pyrophosphate titanium fluorescent material
Chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 8:1.
The weight ratio of embodiment 6: comparative example, ammonium hydrogen phosphate and natrium nitrosum is 5:1
Chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 5:1.
The weight ratio of embodiment 7: comparative example, ammonium hydrogen phosphate and natrium nitrosum is 9:1
Chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 9:1.
Embodiment 8: effect example
The luminescent properties of the fluorescent material of testing example 1～7 preparation respectively, the excitation and emission spectra of different embodiment fluorescent material
Position is basically identical, but luminous intensity, stability of photoluminescence and dispersiveness have relatively big difference, result such as table 1.Wherein, luminous strong
Degree, on the basis of embodiment 1, is set to 100, and remaining embodiment is the relative luminous intensity relative to embodiment 1.
The luminescent properties of the different embodiment fluorescent material of table 1 and dispersiveness
| Luminous intensity | Stability of photoluminescence | Dispersiveness | |
| Embodiment 1 | 100 | Highly stable | Dispersiveness is the best |
| Embodiment 4 | 97 | More stable | Dispersiveness is preferably |
| Embodiment 5 | 98 | More stable | Dispersiveness is preferably |
| Embodiment 6 | 66 | Unstable | Poor dispersion |
| Embodiment 7 | 62 | Unstable | Poor dispersion |
The test result of embodiment 2,3 is basically identical with embodiment 4,5.
Above-mentioned test result indicate that, the calcium pyrophosphate titanium light-emitting phosphor intensity that the present invention provides is high, and stability is high, these advantages
Relevant with the weight ratio of ammonium hydrogen phosphate in flux and natrium nitrosum, when the weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 6～8:1,
Luminous intensity is the highest.
The effect of above-described embodiment indicates that the essentiality content of the present invention, but does not limit protection scope of the present invention with this.
It will be understood by those within the art that, technical scheme can be modified or equivalent, and not take off
Essence and protection domain from technical solution of the present invention.
Claims (5)
1. a LED calcium pyrophosphate titanium fluorescent material, its chemical composition is Ca2-xTi(P2O7)2:xEu2+；Wherein, x value
0.04～0.20, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.04～0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in reducing atmosphere and 1400～1600 DEG C of conditions in high temperature furnace
Lower sintering 4～6 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.7～0.9% of raw material weight, and described flux is the mixed of ammonium hydrogen phosphate and natrium nitrosum
The weight ratio of compound, ammonium hydrogen phosphate and natrium nitrosum is 6～8:1.
LED calcium pyrophosphate titanium fluorescent material the most according to claim 1, its chemical composition is Ca2-xTi(P2O7)2:xEu2+；
Wherein, x value 0.10, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.10；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 7:1.
LED calcium pyrophosphate titanium fluorescent material the most according to claim 1, its chemical composition is Ca2-xTi(P2O7)2:xEu2+；
Wherein, x value 0.04, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.04；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1400 DEG C
Tie 6 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 6:1.
LED calcium pyrophosphate titanium fluorescent material the most according to claim 1, its chemical composition is Ca2-xTi(P2O7)2:xEu2+；
Wherein, x value 0.20, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xEu2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and europium oxide, wherein, x value 0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1600 DEG C
Tie 4 hours, cool down and i.e. obtain described calcium pyrophosphate titanium fluorescent material；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixture of ammonium hydrogen phosphate and natrium nitrosum,
The weight ratio of ammonium hydrogen phosphate and natrium nitrosum is 8:1.
5. according to the arbitrary described LED calcium pyrophosphate titanium fluorescent material of Claims 1 to 4, it is characterised in that: described reducing atmosphere
For Carbon monoxide reduction atmosphere.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02173182A (en) * | 1988-12-27 | 1990-07-04 | Nichia Chem Ind Ltd | Fluorescent lamp emitting light of pink color |
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- 2016-06-27 CN CN201610481308.1A patent/CN105925263A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02173182A (en) * | 1988-12-27 | 1990-07-04 | Nichia Chem Ind Ltd | Fluorescent lamp emitting light of pink color |
Non-Patent Citations (2)
| Title |
|---|
| TAE-GON KIM, ET AL.: "Energy Transfer and Brightness Saturation in (Sr,Ca)2P2O7:Eu2+,Mn2+ Phosphor for UV-LED Lighting", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》 * |
| 洪广言: "《稀土发光材料--基础与应用》", 30 April 2011, 科学出版社 * |
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