CN102191056B - Silicate red luminescent material and preparation method thereof - Google Patents
Silicate red luminescent material and preparation method thereof Download PDFInfo
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- CN102191056B CN102191056B CN 201010123462 CN201010123462A CN102191056B CN 102191056 B CN102191056 B CN 102191056B CN 201010123462 CN201010123462 CN 201010123462 CN 201010123462 A CN201010123462 A CN 201010123462A CN 102191056 B CN102191056 B CN 102191056B
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Abstract
The invention discloses a silicate red luminescent material and a preparation method thereof. The chemical formula of the luminescent material is M(Ln1-xEux)4(SiO4)3O, wherein M may be Ca, Sr or Ba; Ln may be at least one of Y, La and Gd; and x ranges from 0.005 to 0.50. The preparation method comprises: weighing the raw materials according to a ratio, wherein excessive Si raw material is prepared; adding a certain amount of fluxing agent; sintering at a low temperature and calcining at 900 to 1,300 DEG C; and cooling to obtain the silicate red luminescent material. The preparation method of the invention is simple in process and low in cost; and the prepared silicate red luminescent material emits red light under a condition of a wavelength of 610 nanometers, and the purity of the color is high.
Description
Technical field
The present invention relates to the luminescent material technical field, relate in particular to a kind of silicate red illuminating material and preparation method thereof.
Background technology
Compare with LCD display with traditional CRT monitor, plasma flat-panel display (PDP) has advantages such as the visual angle is wide, big area, response is fast, colour reproduction is good, can be made into the indicating meter of large-size.Compare with low pressure mercury lamp with traditional high voltage mercury lamp, non-mercury florescent lamp meets environmental protection ideas more because it does not contain the mercury poisonous to human body.In PDP and non-mercury florescent lamp, fluorescent material is one of key factor of its performance of restriction.
Present widely used three primary colors fluorescent powder mainly contains rouge and powder Y
2O
3: Eu
3+, (Y, Gd) BO
3: Eu
3+, green powder Zn
2SiO
4: Mn
2+, BaAl
12O
19: Mn
2+With blue powder BaMgAl
10O
17: Eu
2+, for rouge and powder Y wherein
2O
3: Eu
3+, because the Eu in the fluorescent material
3+Be in the symmetry centre case, launch wavelength and be positioned near the ruddiness of 600nm, purity of color is relatively poor.
Summary of the invention
The technical problem to be solved in the present invention is, at the above-mentioned defective of prior art, provides a kind of silicate red illuminating material of high color purity.
The technical problem that the present invention further will solve is, the preparation method of a kind of technology silicate red illuminating material simple, with low cost is provided.
In order to reach above-mentioned purpose, according to a first aspect of the present invention, provide a kind of silicate red illuminating material, its chemical formula is M (Ln
1-xEu
x)
4(SiO
4)
3O, wherein, M is Ca, Sr or Ba, and Ln is at least a among Y, La, the Gd, and the span of x is 0.005≤x≤0.50.
In silicate red illuminating material of the present invention, the span of described x is preferably 0.025≤x≤0.25.
In order to reach above-mentioned purpose, according to a second aspect of the present invention, provide a kind of preparation method of silicate red illuminating material, may further comprise the steps:
1. be raw material to contain the M compound, to contain the Ln compound, contain the Eu compound, contain the Si compound, according to the molar ratio of each element in the above-mentioned chemical formula and make and contain the Si compound and take by weighing each raw material by above-mentioned molar ratio excessive 5~30%, and taking by weighing fusing assistant according to the molar ratio 1~10% with above-mentioned chemical formula, ground and mixed evenly forms compound;
2. compound is first 200~700 ℃ of following presintering, then 900~1300 ℃ of calcinings down;
3. step calcinate 2. is cooled to room temperature, namely obtains the silicate red illuminating material.
In the preparation method of silicate red illuminating material of the present invention, preferably, at least a in the oxide compound that the described M of containing compound is M, oxyhydroxide, nitrate, the carbonate, oxide compound or nitrate that the described Ln of containing compound is Ln, oxide compound or nitrate that the described Eu of containing compound is Eu, the described Si of containing compound is silicic acid.
In the preparation method of silicate red illuminating material of the present invention, preferably, described fusing assistant is at least a in boric acid, barium fluoride, the magnesium fluoride.
In the preparation method of silicate red illuminating material of the present invention, preferably, the presintering time of described step in 2. is 2~5h.
In the preparation method of silicate red illuminating material of the present invention, preferably, the calcination time of described step in 2. is 1~24h.
In the preparation method of silicate red illuminating material of the present invention, further preferably, the calcining temperature of described step in 2. is 1000~1200 ℃, and calcination time is 5~10h.
In the preparation method of silicate red illuminating material of the present invention, preferably, 2. described step is: prior to 200~700 ℃ of presintering, cooling presintering product grinds to room temperature with compound, and then in 900~1300 ℃ of calcinings.
Silicate red illuminating material of the present invention is with MLn
4-4x(SiO
4)
3O is matrix, with Eu
3+Be light emitting ionic, its luminescence mechanism is: pass through MLn
4-4x(SiO
4)
3O is that matrix is the strong absorption of the vacuum-ultraviolet light of 150~175nm to wavelength, gives Eu with transmission ofenergy
3+Ion, thus ruddiness launched.
In the silicate red illuminating material of the present invention, when Ln is Gd, at MGd
4-4x(SiO
4)
3After O matrix to wavelength is the strong absorption of vacuum-ultraviolet light of 150~175nm, realize matrix sensitization Gd
3+Highly excited level energy level, and Gd
3+ 6P
JEnergy level and Eu
3+There is transmission ofenergy between the ion, gives Eu with transmission ofenergy
3+Ion has further improved the intensity of launching ruddiness.
In the silicate red illuminating material of the present invention, Eu
3+At MLn
4(SiO
4)
3O (M=Ca, Sr or Ba; At least a among Ln=Y, La, the Gd) be in the case that departs from inversion center of symmetry in the rhombic system, launch wavelength be positioned near the 610nm ruddiness (
5D
0→
7F
2), high color purity, luminous efficiency height have good luminous property.
Among the preparation method of silicate red illuminating material of the present invention, add the raw material that contains the Si element, namely silicic acid is excessive, be in order to obtain pure phase, and because silicic acid can at high temperature volatilize, excessive silicic acid can not remain in the preparation product silicate red illuminating material.
Among the preparation method of silicate red illuminating material of the present invention, one or more in adding boric acid, barium fluoride, the magnesium fluoride can make reaction more abundant, and can reduce the temperature of reaction as fusing assistant.
The preparation method of silicate red illuminating material of the present invention, its technology is simple, product with low cost, the silicate red illuminating material of preparation has good purity of color.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples, in the accompanying drawing:
Fig. 1 is the Ca (Y of the embodiment of the invention 1
0.95Eu
0.05)
4(SiO
4)
3The exciting light spectrogram of O silicate red illuminating material, the monitoring wavelength is 610nm;
Fig. 2 is the Ca (Y of the embodiment of the invention 1
0.95Eu
0.05)
4(SiO
4)
3The emmission spectrum figure of O silicate red illuminating material, excitation wavelength is 172nm;
Fig. 3 is the Ca (Gd of the embodiment of the invention 7
0.975Eu
0.025)
4(SiO
4)
3The exciting light spectrogram of O silicate red illuminating material, the monitoring wavelength is 613nm;
Fig. 4 is the Ca (Gd of the embodiment of the invention 7
0.975Eu
0.025)
4(SiO
4)
3The emmission spectrum figure of O silicate red illuminating material, excitation wavelength is 172m.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples the present invention is further described in detail.
Used rare earths material purity is more than the 4N in the embodiments of the invention, and other raw materials are common commercial goods, and purity is analytical pure.Use for convenience, can be with RE(rare earth) borate luminescent material grind into powder of the present invention.
Embodiment 1
Take by weighing calcium carbonate CaCO
30.3003g, yttrium oxide Y
2O
31.2871g, silicic acid H
2SiO
3(0.7380g excessive 5% according to the molar equivalent of element silicon in the silicate red illuminating material that finally obtains, down with), europium sesquioxide Eu
2O
30.1056g and magnesium fluoride MgF
2(0.0093g the molar ratio of magnesium fluoride and silicate red illuminating material is 5%, and the numerical value in following examples is method of calculation herewith).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 600 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 5h down at 1000 ℃, cooling namely gets Ca (Y after the grinding
0.95Eu
0.05)
4(SiO
4)
3O silicate red illuminating material.
Fig. 1 is the Ca (Y of the embodiment of the invention 1
0.95Eu
0.05)
4(SiO
4)
3The exciting light spectrogram of O silicate red illuminating material, the monitoring wavelength X
EmBe 610nm.Fig. 2 is the Ca (Y of the embodiment of the invention 1
0.95Eu
0.05)
4(SiO
4)
3The emmission spectrum figure of O silicate red illuminating material, excitation wavelength lambda
ExBe 172nm.As seen from Figure 2, the Ca (Y of present embodiment
0.95Eu
0.05)
4(SiO
4)
3O silicate red illuminating material is that the 610nm place launches ruddiness at wavelength, and and Y
2O
3: Eu
3+Red luminescence phosphor is that the ruddiness that the 600nm place launches is compared at wavelength, and purity of color is improved.
Embodiment 2
Take by weighing calcium carbonate CaCO
30.3003g, lanthanum trioxide La
2O
31.8571g, silicic acid H
2SiO
30.7380g europium sesquioxide Eu (5%),
2O
30.1056g and barium fluoride BaF
20.0053g (1%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 600 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 5h down at 1000 ℃, cooling namely gets Ca (La after the grinding
0.95Eu
0.05)
4(SiO
4)
3O silicate red illuminating material.
Embodiment 3
Take by weighing barium carbonate BaCO
30.5920g, yttrium oxide Y
2O
31.2871g, silicic acid H
2SiO
30.7380g europium sesquioxide Eu (5%),
2O
30.1056g and boric acid H
3BO
30.0093g (5%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 600 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 5h down at 1300 ℃, cooling namely gets Ba (Y after the grinding
0.95Eu
0.05)
4(SiO
4)
3O silicate red illuminating material.
Take by weighing barium carbonate BaCO
30.5920g, lanthanum trioxide La
2O
31.8571g, silicic acid H
2SiO
30.7380g europium sesquioxide Eu (5%),
2O
30.1056g and magnesium fluoride MgF
20.0093g (5%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 600 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 5h down at 1300 ℃, cooling namely gets Ba (La after the grinding
0.95Eu
0.05)
4(SiO
4)
3O silicate red illuminating material.
Embodiment 5
Take by weighing Strontium carbonate powder SrCO
30.4429g, yttrium oxide Y
2O
31.2871g, silicic acid H
2SiO
30.7380g europium sesquioxide Eu (5%),
2O
30.1056g and barium fluoride BaF
20.0053g (1%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 600 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 5h down at 1100 ℃, cooling namely gets Sr (Y after the grinding
0.95Eu
0.05)
4(SiO
4)
3O silicate red illuminating material.
Embodiment 6
Take by weighing Strontium carbonate powder SrCO
30.4429g, lanthanum trioxide La
2O
31.8571g, silicic acid H
2SiO
30.7380g europium sesquioxide Eu (5%),
2O
30.1056g and magnesium fluoride MgF
20.0093g, barium fluoride BaF
20.0053g (6%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 600 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 5h down at 1100 ℃, cooling namely gets Sr (La after the grinding
0.95Eu
0.05)
4(SiO
4)
3O silicate red illuminating material.
Embodiment 7
Take by weighing calcium carbonate CaCO
30.3003g, gadolinium sesquioxide Gd
2O
32.1206g, silicic acid H
2SiO
30.7380g europium sesquioxide Eu (5%),
2O
30.0527g and boric acid H
3BO
30.0093g (5%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 500 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 5h down at 1100 ℃, cooling namely gets Ca (Gd after the grinding
0.975Eu
0.025)
4(SiO
4)
3O silicate red illuminating material.
Fig. 3 is the Ca (Gd of the embodiment of the invention 7
0.975Eu
0.025)
4(SiO
4)
3The exciting light spectrogram of O silicate red illuminating material, the monitoring wavelength X
EmBe 613nm.Fig. 4 is the Ca (Gd of the embodiment of the invention 7
0.975Eu
0.025)
4(SiO
4)
3The emmission spectrum figure of O silicate red illuminating material, excitation wavelength lambda
ExBe 172nm.As seen from Figure 4, the Ca (Gd of present embodiment
0.975Eu
0.025)
4(SiO
4)
3O silicate red illuminating material is that the 613nm place launches ruddiness at wavelength, and and Y
2O
3: Eu
3+Red luminescence phosphor is that the ruddiness that the 600nm place launches is compared at wavelength, and purity of color is improved.
Embodiment 8
Take by weighing barium carbonate BaCO
30.5920g, gadolinium sesquioxide Gd
2O
32.1206g, silicic acid H
2SiO
30.7380g europium sesquioxide Eu (5%),
2O
30.0527g and barium fluoride BaF
20.0053g (1%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 500 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, abundant grinding product is calcined 5h down at 1300 ℃ again, and cooling namely gets Ba (Gd after the grinding
0.975Eu
0.025)
4(SiO
4)
3O silicate red illuminating material.
Embodiment 9
Take by weighing Strontium carbonate powder SrCO
30.4429g, gadolinium sesquioxide Gd
2O
32.1206g, silicic acid H
2SiO
30.7380g europium sesquioxide Eu (5%),
2O
30.0527g and magnesium fluoride MgF
20.0093g (5%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 500 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 5h down at 1200 ℃, cooling namely gets Sr (Gd after the grinding
0.975Eu
0.025)
4(SiO
4)
3O silicate red illuminating material.
Embodiment 10
Take by weighing calcium carbonate CaCO
30.3003g, gadolinium sesquioxide Gd
2O
32.0662g, yttrium oxide Y
2O
30.0339g, silicic acid H
2SiO
30.7380g europium sesquioxide Eu (5%),
2O
30.0527g and boric acid H
3BO
30.0093g (5%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 500 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 5h down at 1100 ℃, cooling namely gets Ca (Gd after the grinding
0.95Y
0.025Eu
0.025)
4(SiO
4)
3O red fluorescence luminescent material.
Embodiment 11
Take by weighing calcium oxide CaO 0.1682g, lanthanum trioxide La
2O
31.2967g, silicic acid H
2SiO
30.9138g europium sesquioxide Eu (30%),
2O
30.0106g and barium fluoride BaF
20.0421g (8%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 200 ℃ of following presintering 5h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 24h down at 900 ℃, cooling namely gets Ca (La after the grinding
0.995Eu
0.005)
4(SiO
4)
3O silicate red illuminating material.
Embodiment 12
Take by weighing hydrated barta Ba (OH)
20.5140g, Yttrium trinitrate Y (NO
3)
36H
2O 2.2975g, silicic acid H
2SiO
30.7732g europium nitrate Eu (NO (10%),
3)
36H
2O 2.6759g and boric acid H
3BO
30.0056g (3%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 700 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 1h down at 1300 ℃, cooling namely gets Ba (Y after the grinding
0.50Eu
0.50)
4(SiO
4)
3O silicate red illuminating material.
Embodiment 13
Take by weighing nitrate of baryta Ba (NO
3)
20.7840g, lanthanum nitrate La (NO
3)
36H
2O 4.1560g, silicic acid H
2SiO
30.8435g europium nitrate Eu (NO (20%),
3)
36H
2O 1.0704g and magnesium fluoride MgF
20.0187g (10%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 600 ℃ of following presintering 3h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 10h down at 1000 ℃, cooling namely gets Ba (La after the grinding
0.80Eu
0.20)
4(SiO
4)
3O silicate red illuminating material.
Embodiment 14
Take by weighing barium carbonate BaCO
30.5920g, yttrium oxide Y
2O
31.0161g, silicic acid H
2SiO
30.7380g europium sesquioxide Eu (5%),
2O
30.5279g and boric acid H
3BO
30.0093g (5%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible at 600 ℃ of following presintering 2h, be cooled to room temperature then, take out again and fully grind.At last, the regrinding product is calcined 5h down at 1300 ℃, cooling namely gets Ba (Y after the grinding
0.75Eu
0.25)
4(SiO
4)
3O silicate red illuminating material.
The above only is representative embodiment of the present invention, does not limit the present invention in any way, and all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces or improvement etc., all should be included within protection scope of the present invention.
For example, after all raw materials and fusing assistant presintering at a lower temperature, without regrinding, also be fine 900~1300 ℃ of following calcinings then.
Claims (5)
1. the preparation method of a silicate red illuminating material is characterized in that, may further comprise the steps:
1. be raw material to contain the M compound, to contain the Ln compound, contain the Eu compound, contain the Si compound, according to M (Ln
1-xEu
x)
4(SiO
4)
3The molar ratio of each element and make and contain the Si compound and take by weighing each raw material by above-mentioned molar ratio excessive 5~30% among the O, and according to M (Ln
1-xEu
x)
4(SiO
4)
3The molar ratio 1~10% of O takes by weighing fusing assistant, and ground and mixed evenly forms compound, and wherein, M is Sr or Ba, and Ln is at least a among Y, La, the Gd, and the span of x is 0.005≤x≤0.50; Described fusing assistant is at least a in boric acid, barium fluoride, the magnesium fluoride; At least a in the oxide compound that the described M of containing compound is M, oxyhydroxide, nitrate, the carbonate, oxide compound or nitrate that the described Ln of containing compound is Ln, oxide compound or nitrate that the described Eu of containing compound is Eu, the described Si of containing compound is silicic acid;
2. after compound being placed agate mortar fully to grind, 200~700 ℃ of following presintering, cool off the presintering product then to room temperature, fully grind again, at last 900~1300 ℃ of calcinings down;
3. step calcinate 2. is cooled to room temperature, namely obtains the silicate red illuminating material after the grinding.
2. the preparation method of silicate red illuminating material according to claim 1 is characterized in that, the span of described x is 0.025≤x≤0.25.
3. the preparation method of silicate red illuminating material according to claim 1 is characterized in that, the presintering time of described step in 2. is 2~5h.
4. the preparation method of silicate red illuminating material according to claim 1 is characterized in that, the calcination time of described step in 2. is 1~24h.
5. the preparation method of silicate red illuminating material according to claim 4 is characterized in that, the calcining temperature of described step in 2. is 1000~1200 ℃, and calcination time is 5~10h.
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CN108659840A (en) * | 2018-07-25 | 2018-10-16 | 淮阴师范学院 | Eu3+Red fluorescence powder of activation and preparation method thereof |
CN111410958B (en) * | 2020-05-21 | 2023-01-31 | 哈尔滨工业大学 | Method for preparing red fluorescent powder by using LiF as fluxing agent |
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CN1470597A (en) * | 2003-07-07 | 2004-01-28 | 中国科学院长春应用化学研究所 | Method for preparing silicate light-emitting film |
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Non-Patent Citations (2)
Title |
---|
Ca(La1-xEux)Si3O13 red emitting phosphor for white light emitting diodes;Changyu Shen et al;《Physica B》;20091231;第404卷;第1481-1484页 * |
Changyu Shen et al.Ca(La1-xEux)Si3O13 red emitting phosphor for white light emitting diodes.《Physica B》.2009,第404卷第1481-1484页. |
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