CN105925264A - Manganese ion-doped calcium pyrophosphate titanium fluorescent powder and preparation method thereof - Google Patents
Manganese ion-doped calcium pyrophosphate titanium fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a manganese ion-doped calcium pyrophosphate titanium fluorescent powder and a preparation method thereof. The chemical composition of the fluorescent powder is Ca2xTi(P2O7)2:xMn<2+>, wherein x is 0.04-0.20. The manganese ion-doped calcium pyrophosphate titanium fluorescent powder is prepared according to the following steps of: S1) weighting the mixture of raw materials, namely calcium carbonate, titanium dioxide, sodium pyrophosphate and manganese nitrate according to the stoichiometric ratio of Ca2xTi(P2O7)2:xMn<2+>, wherein x is 0.04-0.20; S2) adding fluxing agent for grinding, uniformly grinding and acquiring a mixture; and S3) filling the mixture acquired from the step 2) into a crucible, sintering for 4-6 hours in a high temperature furnace under the conditions of reducing atmosphere and 1400-1600 DEG C and cooling, thereby acquiring the product, wherein the adding amount of the fluxing agent is 0.7-09% of the weight of the raw materials, the fluxing agent is the mixture of ammonium sulfide and sodium nitrite and the weight ratio of ammonium sulfide to sodium nitrite is (6-8):1. The manganese ion-doped calcium pyrophosphate titanium fluorescent powder provided by the invention is high in light intensity and high in stability; the advantages are related to the weight ratio of ammonium sulfide and sodium nitrite in the fluxing agent; the light intensity is the highest when the weight ratio of ammonium sulfide and sodium nitrite is (6-8):1.
Description
Technical field
The invention belongs to field of light emitting materials, calcium pyrophosphate titanium fluorescent material being specifically related to a kind of doped with manganese ion 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 electric filament lamp), and colour temperature is
2500K-6500K, color 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
Calcium pyrophosphate titanium fluorescent material that it is an object of the invention to provide a kind of doped with manganese ion and preparation method thereof.
The above-mentioned purpose of the present invention is achieved by techniques below scheme:
The calcium pyrophosphate titanium fluorescent material of a kind of doped with manganese ion, its chemical composition is Ca2-xTi(P2O7)2:xMn2+；Wherein, x value
0.04～0.20, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 mixing of ammonium sulfide and sodium nitrite
The weight ratio of thing, ammonium sulfide and sodium nitrite is 6～8:1.
Further, the calcium pyrophosphate titanium fluorescent material of described doped with manganese ion, its chemical composition is Ca2-xTi(P2O7)2:xMn2+；
Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 7:1.
Further, the calcium pyrophosphate titanium fluorescent material of described doped with manganese ion, its chemical composition is Ca2-xTi(P2O7)2:xMn2+；
Wherein, x value 0.04, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 6:1.
Further, the calcium pyrophosphate titanium fluorescent material of described doped with manganese ion, its chemical composition is Ca2-xTi(P2O7)2:xMn2+；
Wherein, x value 0.20, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite 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 sulfide in flux and
The weight ratio of sodium nitrite is relevant, and when the weight ratio of ammonium sulfide and sodium nitrite 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:xMn2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 7:1.
Embodiment 2: the preparation of calcium pyrophosphate titanium fluorescent material
Chemical composition is Ca2-xTi(P2O7)2:xMn2+；Wherein, x value 0.04, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 6:1.
Embodiment 3: the preparation of calcium pyrophosphate titanium fluorescent material
Chemical composition is Ca2-xTi(P2O7)2:xMn2+；Wherein, x value 0.20, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 8:1.
Embodiment 4: the preparation of calcium pyrophosphate titanium fluorescent material
Chemical composition is Ca2-xTi(P2O7)2:xMn2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 6:1.
Embodiment 5: the preparation of calcium pyrophosphate titanium fluorescent material
Chemical composition is Ca2-xTi(P2O7)2:xMn2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 8:1.
The weight ratio of embodiment 6: comparative example, ammonium sulfide and sodium nitrite is 5:1
Chemical composition is Ca2-xTi(P2O7)2:xMn2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 5:1.
The weight ratio of embodiment 7: comparative example, ammonium sulfide and sodium nitrite is 9:1
Chemical composition is Ca2-xTi(P2O7)2:xMn2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Ca2-xTi(P2O7)2:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite 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 dispersibility 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 dispersibility
| Luminous intensity | Stability of photoluminescence | Dispersibility | |
| Embodiment 1 | 100 | Highly stable | Dispersibility is the best |
| Embodiment 4 | 97 | More stable | Dispersibility is preferable |
| Embodiment 5 | 98 | More stable | Dispersibility is preferable |
| Embodiment 6 | 66 | Unstable | Poor dispersion |
| Embodiment 7 | 67 | Unstable | Poor dispersion |
The test result of embodiment 2,3 is basically identical with embodiment 4,5.
Result shows, the calcium pyrophosphate titanium light-emitting phosphor intensity that the present invention provides is high, and stability is high, these advantages and flux
Middle ammonium sulfide is relevant with the weight ratio of sodium nitrite, and when the weight ratio of ammonium sulfide and sodium nitrite 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 calcium pyrophosphate titanium fluorescent material for doped with manganese ion, its chemical composition is Ca2-xTi(P2O7)2:xMn2+；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:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 mixing of ammonium sulfide and sodium nitrite
The weight ratio of thing, ammonium sulfide and sodium nitrite is 6～8:1.
Calcium pyrophosphate titanium fluorescent material the most according to claim 1, its chemical composition is Ca2-xTi(P2O7)2:xMn2+；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:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 7:1.
Calcium pyrophosphate titanium fluorescent material the most according to claim 1, its chemical composition is Ca2-xTi(P2O7)2:xMn2+；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:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 6:1.
Calcium pyrophosphate titanium fluorescent material the most according to claim 1, its chemical composition is Ca2-xTi(P2O7)2:xMn2+；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:xMn2+Stoichiometric proportion weigh raw material, described raw material be calcium carbonate,
The mixture of titanium dioxide, sodium pyrophosphate and manganese nitrate, 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 sulfide and sodium nitrite,
The weight ratio of ammonium sulfide and sodium nitrite is 8:1.
5. according to the calcium pyrophosphate titanium fluorescent material of the arbitrary described doped with manganese ion of Claims 1 to 4, it is characterised in that: described also
Primordial Qi atmosphere is 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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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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Application publication date: 20160907 |