CN101717638A - Fluorescent powder for field emission and method for preparing same - Google Patents
Fluorescent powder for field emission and method for preparing same Download PDFInfo
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- CN101717638A CN101717638A CN200910217921A CN200910217921A CN101717638A CN 101717638 A CN101717638 A CN 101717638A CN 200910217921 A CN200910217921 A CN 200910217921A CN 200910217921 A CN200910217921 A CN 200910217921A CN 101717638 A CN101717638 A CN 101717638A
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Abstract
The invention relates to fluorescent powder for field emission and a method for preparing the same. The fluorescent powder for the field emission has a chemical formula A1-xSi2O2N2:Eux, wherein x is greater than 0 and is not greater than 0.2; and A is at least one of Ba and Sr which are of any mol ratio. The method comprises the following steps: selecting carbonate, nitride and oxide as raw materials and adding 0 to 5 mol percent of latent solvent into the raw materials for mixing; sintering the mixture at 1,200 DEG C for 2 hours under a reducing condition or in nitrogen; and sintering the mixture at 1,500 to 1,550 DEG C for 2 to 6 hours under the reducing condition or in the nitrogen; and cooling the sintered mixture to obtain the fluorescent powder for the field emission. The fluorescent powder for the field emission prepared by the method has the characteristics of emission distance variable between 490 and 532 nanometers, fluorescent lifetime of 0.50 microseconds and 0.77 microseconds and 91 percent fluorescence quantum efficiency, and compared with commercial ZnO:Zn, has higher color purity.
Description
Technical field
The present invention relates to a kind of fluorescent powder for field emission and preparation method thereof.
Background technology
Field Emission Display (FED) is the flat-panel monitor that a kind of new development is got up, its principle of work and traditional cathode tube are similar, is imaging by the fluorescent material on the beam bombardment display screen.Compare with other flat-panel monitor (FPD), FED all has the potential advantage at aspects such as brightness, visual angle, time of response, operating temperature range, energy consumptions.One of key factor of preparation premium properties FED is the preparation of fluorescent material.The fluorescent material that adopts mainly is some fluorescent material that are used for conventional cathode x ray tube and projection TV picture tube at present: blue powder ZnS:Ag, Cl, SrGa
2S
4: Ce[reference Zhang F.L., Yang S., Stoffers C., Appl.Phys.Lett., 72,2226 (1998)], Y
2SiO
5: Ce[reference Lee R.Y., Kim S.W., J.Lumin., 93,93 (2001)]; Green powder SrGa
2S
4: Eu[reference YangS., Stoffers C.Zhang F., Appl.Phys.Lett., 72,158 (1998)], ZnGa
2O
4: Mn[reference Kim J.Y., Jeon D.Y., Yu L., J.Electrochem.Soc.147,3559 (2000)]; Rouge and powder Y
2O
2S:Eu[reference Shea L.E., Materials ScienceProgram[D] .San Diego, USA:University of California, 1997.], Y
2O
3: Eu[reference Mays R., Measured data[Z] .Sandia, USA:SandiaNational Laboratories, 1997].Sulfide-basedly show higher luminosity, and its less stable, decompose easily under the low-voltage, high-current beam bombardment and produce sulphur, make the performance degradation of material itself on the one hand, sulphur anticathode electron emission pin has serious " poisoning " to act on the other hand.Oxide compound series has advantages of higher stability, but its luminosity is not as sulfide series.Except that the red, green, blue powder, cyan fluorescent material also becomes the research and development focus gradually.Nitride and nitric oxide fluorescent powder cause everybody concern at present.This series phosphor powder has good chemistry and thermostability, can effectively be excited by ultraviolet or blue light.Be expected in white light LEDs, to obtain to use, and they do not appear in the newspapers with fluorescent material as yet as Field Emission Display.
Summary of the invention
One of purpose of the present invention provides a kind of fluorescent powder for field emission.Its chemical formula is:
A
1-xSi
2O
2N
2:Eu
x
Wherein, 0＜x≤0.2; A is at least a of Ba and Sr, and Ba and Sr are any mol ratio.
Two of purpose of the present invention provides the preparation method of described fluorescent powder for field emission, and its step and condition are as follows:
Raw material is the carbonate that contains A, siliceous nitride and oxide compound and the oxide compound that contains europium, and wherein, A is at least a of Ba and Sr;
Fusing assistant is that ammonium chloride, Neutral ammonium fluoride and boric acid are at least a;
Press chemical formula A
1-xSi
2O
2N
2: Eu
xStoichiometric ratio take by weighing raw material, add fusing assistant again and carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, then under reducing atmosphere or nitrogen in 1200 ℃ of sintering 2 hours, again under reducing atmosphere or nitrogen in 1500～1550 ℃ of sintering 2-6 hours, be cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission; Described reducing atmosphere is that volume ratio is 1～5%: 99～95% H
2And N
2Mixed gas; The mole number of described fusing assistant and chemical formula A
1-xSi
2O
2N
2: Eu
xThe ratio of total mole number be 0～5%: 1.
Beneficial effect: the fluorescent powder for field emission of the present invention's preparation is transmitted between 490 and 532 nanometers and can changes.Fluorescence lifetime is 0.50 and 0.77 microsecond (see figure 2).Luminous quantum efficiency reaches 91%.With commercial ZnO: Zn compares, and has higher purity of color (see figure 3).
Description of drawings
Fig. 1 is the low pressure (exciting voltage: 3.0kV) negative ray spectrogram of fluorescent powder for field emission.Wherein, curve (a) is the fluorescent powder for field emission of embodiment a 5 (exciting voltage: 3.0kV) negative ray spectrogram; Curve (b) is (exciting voltage: 3.0kV) negative ray spectrogram of the fluorescent powder for field emission of embodiment 17.
Fig. 2 curve (A) is embodiment 5 fluorescence lifetime curves, and fluorescence lifetime is 0.77 microsecond; Curve (B) is the fluorescence lifetime curve of embodiment 17, and fluorescence lifetime is 0.50 microsecond.
It is the chromaticity coordinates of the fluorescent powder for field emission of embodiment 5 that Fig. 3 is at 1, wherein, and x=0.14; Y=0.35; 2 is the chromaticity coordinates of the fluorescent powder for field emission of embodiment 17, wherein, and x=0.28; Y=0.57.3 is the chromaticity coordinates of commercial fluorescent powder Zn O:Zn, wherein, and x=0.25; Y=0.45.
Embodiment
Embodiment 1
Under the room temperature, take by weighing BaCO
30.5861 gram, Si
3N
40.2806 gram, Eu
2O
30.0053 gram carries out abundant ground and mixed, puts into corundum crucible, puts into High Temperature Furnaces Heating Apparatus, at N
2Under the atmosphere in 1200 ℃ of sintering 2 hours, again in 1500 ℃ of N
2Calcining is 2 hours under the atmosphere, and products therefrom is cooled to room temperature, places mortar to grind evenly, obtains fluorescent powder for field emission, and it consists of Ba
0.99Si
2O
2N
2: Eu
2+ 0.01
Under the room temperature, take by weighing BaCO
30.5802 gram, Si
3N
40.2806 gram, Eu
2O
30.0106 gram carries out abundant ground and mixed, puts into corundum crucible, puts into High Temperature Furnaces Heating Apparatus, at N
2Under the atmosphere in 1200 ℃ of sintering 2 hours, again in 1500 ℃ of N
2Calcining is 2 hours under the atmosphere, and products therefrom is cooled to room temperature, places mortar to grind evenly, obtains fluorescent powder for field emission, and it consists of Ba
0.98Si
2O
2N
2: Eu
2+ 0.02
Embodiment 3
Under the room temperature, take by weighing BaCO
30.5742 gram, Si
3N
40.2806 gram, Eu
2O
30.0158 gram carries out abundant ground and mixed, puts into corundum crucible, puts into High Temperature Furnaces Heating Apparatus, at N
2Under the atmosphere in 1200 ℃ of sintering 2 hours, again in 1500 ℃ of N
2Calcining is 2 hours under the atmosphere, and products therefrom is cooled to room temperature, places mortar to grind evenly, obtains fluorescent powder for field emission, and it consists of Ba
0.97Si
2O
2N
2: Eu
2+ 0.03
Embodiment 4
Under the room temperature, take by weighing BaCO
30.5683 gram, Si
3N
40.2806 gram, Eu
2O
30.0211 gram carries out abundant ground and mixed, puts into corundum crucible, puts into High Temperature Furnaces Heating Apparatus, at N
2Under the atmosphere in 1200 ℃ of sintering 2 hours, again in 1500 ℃ of N
2Calcining is 2 hours under the atmosphere, and products therefrom is cooled to room temperature, places mortar to grind evenly, obtains fluorescent powder for field emission, and it consists of Ba
0.96Si
2O
2N
2: Eu
2+ 0.04
Embodiment 5
Under the room temperature, take by weighing BaCO
30.5624 gram, Si
3N
40.2806 gram, Eu
2O
30.0264 gram carries out abundant ground and mixed, puts into corundum crucible, puts into High Temperature Furnaces Heating Apparatus, at N
2Under the atmosphere in 1200 ℃ of sintering 2 hours, again in 1500 ℃ of N
2Calcining is 2 hours under the atmosphere, and products therefrom is cooled to room temperature, places mortar to grind evenly, obtains fluorescent powder for field emission, and it consists of Ba
0.95Si
2O
2N
2: Eu
2+ 0.05
Embodiment 6
Under the room temperature, take by weighing BaCO
30.5565 gram, Si
3N
40.2806 gram, Eu
2O
30.0317 gram carries out abundant ground and mixed, puts into corundum crucible, puts into High Temperature Furnaces Heating Apparatus, at N
2Under the atmosphere in 1200 ℃ of sintering 2 hours, again in 1500 ℃ of N
2Calcining is 2 hours under the atmosphere, and products therefrom is cooled to room temperature, places mortar to grind evenly, obtains fluorescent powder for field emission, and it consists of Ba
0.94Si
2O
2N
2: Eu
2+ 0.06
Embodiment 7
Under the room temperature, take by weighing BaCO
30.5506 gram, Si
3N
40.2806 gram, Eu
2O
30.0370 gram carries out abundant ground and mixed, puts into corundum crucible, puts into High Temperature Furnaces Heating Apparatus, at N
2Under the atmosphere in 1200 ℃ of sintering 2 hours, again in 1500 ℃ of N
2Calcining is 2 hours under the atmosphere, and products therefrom is cooled to room temperature, places mortar to grind evenly, obtains fluorescent powder for field emission, and it consists of Ba
0.93Si
2O
2N
2: Eu
2+ 0.07
Embodiment 8
Under the room temperature, take by weighing BaCO
30.5446 gram, Si
3N
40.2806 gram, Eu
2O
30.0422 gram carries out abundant ground and mixed, puts into corundum crucible, puts into High Temperature Furnaces Heating Apparatus, at N
2Under the atmosphere in 1200 ℃ of sintering 2 hours, again in 1500 ℃ of N
2Calcining is 2 hours under the atmosphere, and products therefrom is cooled to room temperature, places mortar to grind evenly, obtains fluorescent powder for field emission, and it consists of Ba
0.92Si
2O
2N
2: Eu
2+ 0.08
Embodiment 9
Under the room temperature, take by weighing BaCO
30.5387 gram, Si
3N
40.2806 gram, Eu
2O
30.0475 gram carries out abundant ground and mixed, puts into corundum crucible, puts into High Temperature Furnaces Heating Apparatus, at N
2Under the atmosphere in 1200 ℃ of sintering 2 hours, again in 1500 ℃ of N
2Calcining is 2 hours under the atmosphere, and products therefrom is cooled to room temperature, places mortar to grind evenly, obtains fluorescent powder for field emission, and it consists of Ba
0.91Si
2O
2N
2: Eu
2+ 0.09
Under the room temperature, take by weighing BaCO
30.5328 gram, Si
3N
40.2806 gram, Eu
2O
30.0528 gram carries out abundant ground and mixed, puts into corundum crucible, puts into High Temperature Furnaces Heating Apparatus, at N
2Under the atmosphere in 1200 ℃ of sintering 2 hours, again in 1500 ℃ of N
2Calcining is 2 hours under the atmosphere, and products therefrom is cooled to room temperature, places mortar to grind evenly, obtains fluorescent powder for field emission, and it consists of Ba
0.90Si
2O
2N
2: Eu
2+ 0.10
Embodiment 11
Under the room temperature, take by weighing BaCO
30.5624 gram, Si
3N
40.2806 gram, Eu
2O
30.0264 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 2 hours down of 1500 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Ba
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 1%: 99% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 12
Under the room temperature, take by weighing BaCO
30.5624 gram, Si
3N
40.2806 gram, Eu
2O
30.0264 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 2 hours down of 1500 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Ba
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 13
Under the room temperature, take by weighing BaCO
30.5624 gram, Si
3N
40.2806 gram, Eu
2O
30.0264 gram adds fusing assistant NH again
4Cl 0.0048 gram carries out abundant ground and mixed, total mole ratio of the mole number of described fusing assistant and the chemical constitution formula of described fluorescent material is 3%, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 2 hours down of 1500 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Ba
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 14
Under the room temperature, take by weighing BaCO
30.5624 gram, Si
3N
40.2806 gram, Eu
2O
30.0264 gram, NH
4F 0.0033 gram carries out abundant ground and mixed, total mole ratio of the mole number of described fusing assistant and the chemical constitution formula of described fluorescent material is 3%, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 2 hours down of 1500 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Ba
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 15
Under the room temperature, take by weighing BaCO
30.5624 gram, Si
3N
40.2806 gram, Eu
2O
30.0264 gram, H
3BO
30.0056 gram carries out abundant ground and mixed, total mole ratio of the mole number of described fusing assistant and the chemical constitution formula of described fluorescent material is 3%, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 2 hours down of 1500 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Ba
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 16
Under the room temperature, take by weighing BaCO
30.5624 gram, SiO
20.0361 gram, Si
3N
40.2520 gram, Eu
2O
30.0264 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 2 hours down of 1500 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Ba
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 17
Under the room temperature, take by weighing SrCO
30.7012 gram, Si
3N
40.4770 gram, Eu
2O
30.0440 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 2 hours down of 1550 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 18
Under the room temperature, take by weighing SrCO
30.6643 gram, Si
3N
40.4770 gram, Eu
2O
30.0880 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 2 hours down of 1550 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.90Si
2O
2N
2: Eu
2+ 0.10Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 19
Under the room temperature, take by weighing SrCO
30.5905 gram, Si
3N
40.4770 gram, Eu
2O
30.1760 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 2 hours down of 1550 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.80Si
2O
2N
2: Eu
2+ 0.20Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 20
Under the room temperature, take by weighing SrCO
30.7012 gram, SiO
20.0601 gram, Si
3N
40.4770 gram, Eu
2O
30.0440 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 2 hours down of 1550 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 21
Under the room temperature, take by weighing SrCO
30.7012 gram, Si
3N
40.4200 gram, Eu
2O
30.0440 gram, NH
4Cl 0.0081 gram, the mole number of described fusing assistant is 5% with the total mole number ratio of the chemical constitution formula of described fluorescent material, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, calcined 2 hours down in 1550 ℃ of reducing atmospheres again, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 22
Under the room temperature, take by weighing SrCO
30.7012 gram, Si
3N
40.4200 gram, Eu
2O
30.0440 gram, NH
4F 0.0056 gram, the mole number of described fusing assistant is 3% with the total mole number ratio of the chemical constitution formula of described fluorescent material, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, calcined 2 hours down in 1550 ℃ of reducing atmospheres again, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 23
Under the room temperature, take by weighing SrCO
30.7012 gram, Si
3N
40.4200 gram, Eu
2O
30.0440 gram, H
3BO
30.0093 gram, the mole number of described fusing assistant is 3% with the total mole number ratio of the chemical constitution formula of described fluorescent material, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, calcined 2 hours down in 1550 ℃ of reducing atmospheres again, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.95Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 24
Under the room temperature, take by weighing SrCO
30.3691 gram, BaCO
30.4440 gram, Si
3N
40.4200 gram, Eu
2O
30.0440 gram, H
3BO
30.0093 gram, the mole number of described fusing assistant is 3% with the total mole number ratio of the chemical constitution formula of described fluorescent material, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, calcined 2 hours down in 1550 ℃ of reducing atmospheres again, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.50Ba
0.45Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 25
Under the room temperature, take by weighing SrCO
30.3691 gram, BaCO
30.4440 gram, Si
3N
40.4200 gram, Eu
2O
30.0440 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 6 hours down of 1550 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.50Ba
0.45Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 26
Under the room temperature, take by weighing SrCO
30.3691 gram, BaCO
30.4440 gram, Si
3N
40.4200 gram, Eu
2O
30.0440 gram, NH
4Cl 0.0048 gram, NH
4F 0.0022 gram, the mole number of described fusing assistant is 5% with the total mole number ratio of the chemical constitution formula of described fluorescent material, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, calcined 6 hours down in 1550 ℃ of reducing atmospheres again, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.50Ba
0.45Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 27
Under the room temperature, take by weighing SrCO
30.3691 gram, BaCO
30.4440 gram, Si
3N
40.4200 gram, Eu
2O
30.0440 gram, NH
4Cl 0.0048 gram, H
3BO
30.0037 gram, the mole number of described fusing assistant is 5% with the total mole number ratio of the chemical constitution formula of described fluorescent material, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, calcined 6 hours down in 1550 ℃ of reducing atmospheres again, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.50Ba
0.45Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 28
Under the room temperature, take by weighing SrCO
30.3691 gram, BaCO
30.4440 gram, Si
3N
40.4200 gram, Eu
2O
30.0440 gram, NH
4F 0.0033 gram, H
3BO
30.0048 gram, the mole number of described fusing assistant is 5% with the total mole number ratio of the chemical constitution formula of described fluorescent material, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, calcined 6 hours down in 1550 ℃ of reducing atmospheres again, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.50Ba
0.45Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 29
Under the room temperature, take by weighing SrCO
30.3691 gram, BaCO
30.4440 gram, Si
3N
40.4200 gram, Eu
2O
30.4770 gram, NH
4Cl 0.0016 gram, NH
4F 0.0033 gram, H
3BO
30.0048 gram, the mole number of described fusing assistant is 5% with the total mole number ratio of the chemical constitution formula of described fluorescent material, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, calcined 6 hours down in 1550 ℃ of reducing atmospheres again, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.50Ba
0.45Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 30
Under the room temperature, take by weighing SrCO
30.0369 gram, BaCO
30.8880 gram, Si
3N
40.4200 gram, Eu
2O
30.0440 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 6 hours down of 1550 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Ba
0.90Sr
0.05Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 31
Under the room temperature, take by weighing SrCO
30.6642 gram, BaCO
30.0493 gram, Si
3N
40.4200 gram, Eu
2O
30.0440 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 6 hours down of 1550 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.90Ba
0.05Si
2O
2N
2: Eu
2+ 0.05Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Embodiment 32
Under the room temperature, take by weighing SrCO
30.5535 gram, BaCO
30.0493 gram, Si
3N
40.4200 gram, Eu
2O
30.1760 gram, carry out abundant ground and mixed, put into corundum crucible, put into High Temperature Furnaces Heating Apparatus, under reducing atmosphere in 1200 ℃ of sintering 2 hours, again in the calcining 6 hours down of 1550 ℃ of reducing atmospheres, products therefrom is cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission, it consists of Sr
0.75Ba
0.05Si
2O
2N
2: Eu
2+ 0.20Described reducing atmosphere is that volume ratio is 5%: 95% H
2And N
2Mixed gas is a reaction atmosphere.
Claims (2)
1. fluorescent powder for field emission is characterized in that, its chemical formula is:
A
1-xSi
2O
2N
2:Eu
x
Wherein, 0＜x≤0.2; A is at least a of Ba and Sr, and Ba and Sr are any mol ratio.
2. the preparation method of fluorescent powder for field emission as claimed in claim 1 is characterized in that, step and condition are as follows:
Raw material is the carbonate that contains A, siliceous nitride and oxide compound and the oxide compound that contains europium, and wherein, A is at least a of Ba and Sr;
Fusing assistant is that ammonium chloride, Neutral ammonium fluoride and boric acid are at least a;
Press chemical formula A
1-xSi
2O
2N
2: Eu
xStoichiometric ratio take by weighing raw material, add fusing assistant again and mix; The mole number of described fusing assistant and chemical formula A
1-xSi
2O
2N
2: Eu
xThe ratio of total mole number be 0～5%: 1, then under reducing atmosphere or nitrogen in 1200 ℃ of sintering 2 hours, again under reducing atmosphere or nitrogen in 1500～1550 ℃ of sintering 2-6 hours, be cooled to room temperature, place mortar to grind evenly, obtain fluorescent powder for field emission; Described reducing atmosphere is that volume ratio is 1～5%: 99～95% H
2And N
2Mixed gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910217921A CN101717638A (en) | 2009-11-26 | 2009-11-26 | Fluorescent powder for field emission and method for preparing same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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Publications (1)
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|---|---|
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Family
ID=42432281
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977882A (en) * | 2012-12-27 | 2013-03-20 | 重庆市科学技术研究院 | Metal silicon-based nitrogen oxide fluorescent powder and preparation method thereof |
| CN105273713A (en) * | 2014-07-18 | 2016-01-27 | 三星电子株式会社 | Phosphor and method of preparing same |
-
2009
- 2009-11-26 CN CN200910217921A patent/CN101717638A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977882A (en) * | 2012-12-27 | 2013-03-20 | 重庆市科学技术研究院 | Metal silicon-based nitrogen oxide fluorescent powder and preparation method thereof |
| CN102977882B (en) * | 2012-12-27 | 2015-04-22 | 重庆市科学技术研究院 | Metal silicon-based nitrogen oxide fluorescent powder and preparation method thereof |
| CN105273713A (en) * | 2014-07-18 | 2016-01-27 | 三星电子株式会社 | Phosphor and method of preparing same |
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