CN103361053A - Silicate luminous material and preparation method thereof - Google Patents

Silicate luminous material and preparation method thereof Download PDF

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Publication number
CN103361053A
CN103361053A CN2012100882489A CN201210088248A CN103361053A CN 103361053 A CN103361053 A CN 103361053A CN 2012100882489 A CN2012100882489 A CN 2012100882489A CN 201210088248 A CN201210088248 A CN 201210088248A CN 103361053 A CN103361053 A CN 103361053A
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luminescent material
sio
silicate luminescent
preparation
source compound
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CN2012100882489A
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周明杰
刘军
王荣
陈贵堂
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Priority to CN2012100882489A priority Critical patent/CN103361053A/en
Publication of CN103361053A publication Critical patent/CN103361053A/en
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Abstract

The invention belongs to the field of luminous materials and discloses a silicate luminous material and a preparation method thereof. The silicate luminous material has a chemical formula of M2Ln8-x(SiO4)6O2:xRE<3+>, wherein M is one or two in elements of Sr, Ba, Mg and Ca; Ln is at least one of elements Y and La; RE is one or two in elements of Tb, Gd, Sm, Eu, Dy, Ce and Tm; x is a stoichiometric coefficient; and x ranges from 0.001 to 0.5. The silicate luminous material disclosed by the invention has high luminous efficiency under electron-beam excitation and can be well applied to a field emission light source device.

Description

A kind of silicate luminescent material and preparation method thereof
Technical field
The present invention relates to luminescent material, relate in particular to a kind of silicate luminescent material and preparation method thereof.
Background technology
Feds is because its running voltage is low in recent years, power consumption is little, do not need deflector coil, without X-radiation, the advantage such as radioprotective and magneticinterference and receiving much concern, field-transmitting cathode and luminescent material can be applied to the fields such as demonstration, various indication and general lighting in conjunction with the field emission light source that can obtain high brightness, high colour developing.
Preparing high performance luminescent material is one of key factor of making the premium properties feds.At present, the luminescent material that adopts of feds mainly is sulfide series, oxide compound is serial and the oxysulfide series phosphor powder.For sulfide and oxysulfide series phosphor powder, luminosity is higher, and has certain electroconductibility, but under the bombardment of large beam deflection, decompose easily, emit elemental sulfur and " poison " the negative electrode needle point, and generate other throw outs and cover phosphor surface, reduced the luminous efficiency of fluorescent material, shortened the work-ing life of feds.Oxide compound, silicate fluorescent powder stability are good, but luminous efficiency is high not enough.
Summary of the invention
One of problem to be solved by this invention is to provide a kind of silicate luminescent material that the luminous efficiency of field emission device can be provided.
Technical scheme of the present invention is as follows:
A kind of silicate luminescent material, its chemical formula is: M 2Ln 8-x(SiO 4) 6O 2: xRE 3+Wherein, M is one or both in Sr, Ba, Mg and the Ca element; Ln is at least a in Y and the La element; RE is one or both in Tb, Gd, Sm, Eu, Dy, Ce and the Tm element; X is stoichiometric coefficient, and the span of x is 0.001～0.5.
Two of problem to be solved by this invention is to provide the preparation method of above-mentioned silicate luminescent material, comprises the steps:
(1), according to chemical formula M 2Ln 8-x(SiO 4) 6O 2: xRE 3+In the stoichiometric ratio of each element, take by weighing the source compound of M, the source compound of Ln, the source compound of RE and the source compound of Si, grind, evenly mix, obtain mixed powder;
(2), in air atmosphere or reducing atmosphere, step (1) is obtained mixed powder at 800～1600 ℃ of lower insulation calcining 1～10h, then be cooled to room temperature, take out calcined material, namely get silicate luminescent material after the grinding, the chemical formula of this silicate luminescent material is M 2Ln 8-x(SiO 4) 6O 2: xRE 3+Wherein,
M is one or both in Sr, Ba, Mg and the Ca element; Ln is at least a in Y and the La element; RE is one or both in Tb, Gd, Sm, Eu, Dy, Ce and the m element; X is stoichiometric coefficient, and the span of x is 0.001～0.5.
Silicate luminescent material provided by the invention under electron-beam excitation, has higher luminous efficiency, can be applied in the field emission light source device preferably.
In addition, preparation method's technique of silicate luminescent material of the present invention is simple, quality product is high, cost is low, can be widely used in the luminescent material manufacturing.
Description of drawings
Fig. 1 is that embodiment 1 makes silicate luminescent material and luminescent material (Zn 2SiO 4: luminescent spectrum comparison diagram Mn); Wherein, curve a represents luminescent material (Zn 2SiO 4: luminosity curve Mn), curve b represent the luminosity curve figure of the silicate luminescent material that embodiment 1 makes.
Embodiment
This a kind of silicate luminescent material that embodiment provides, its chemical formula is: M 2Ln 8-x(SiO 4) 6O 2: xRE 3+, wherein, M is one or both in Sr, Ba, Mg and the Ca element; Ln is at least a in Y and the La element; RE is one or both in Tb, Gd, Sm, Eu, Dy, Ce and the Tm element; X is stoichiometric coefficient, and the span of x is 0.001～0.5.
The method of above-mentioned silicate luminescent material may further comprise the steps:
(1), according to chemical formula M 2Ln 8-x(SiO 4) 6O 2: xRE 3+In the stoichiometric coefficient ratio of each element, take by weighing the source compound of M, the source compound of Ln, the source compound of RE and the source compound of Si, grind, evenly mix, obtain mixed powder;
Preferably, the source compound of M is carbonate or the oxalate of M; The source compound of Ln is oxide compound, acetate, carbonate or the oxalate of Ln; The source compound of RE is oxide compound, acetate, carbonate or the oxalate of RE; The source compound of Si is SiO 2Or H 2SiO 3
(2), in air atmosphere or reducing atmosphere, step (1) is obtained mixed powder at 800～1600 ℃ of lower insulation calcining 1～10h, then be cooled to room temperature, take out calcined material, namely get silicate luminescent material after the grinding, the chemical formula of this silicate luminescent material is M 2Ln 8-x(SiO 4) 6O 2: xRE 3+
Preferably, reducing atmosphere is that volume ratio is 95: 5 N 2And H 2Mixed atmosphere;
In the above steps, M is one or both in Sr, Ba, Mg and the Ca element; Ln is at least a in Y and the La element; RE is one or both in Tb, Gd, Sm, Eu, Dy, Ce and the m element; X is stoichiometric coefficient, and the span of x is 0.001～0.5.
Silicate luminescent material provided by the invention under electron-beam excitation, has higher luminous efficiency, can be applied in the field emission light source device preferably.
In addition, preparation method's technique of silicate luminescent material of the present invention is simple, quality product is high, cost is low, can be widely used in the luminescent material manufacturing.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
Sr 2La 7.9(SiO 4) 6O 2:0.1Tb 3+
The total mass number that takes by weighing respectively is the SrCO of 2.9526g, 12.8695g, 3.6051g, 0.1869g 3, La 2O 3, SiO 2, Tb 4O 7Place agate mortar, after the grinding evenly, obtain mixed powder, then mixed powder is put into corundum crucible; Subsequently corundum crucible being placed volume ratio is 95: 5 N 2And H 2In the reducing atmosphere that forms, at 1400 ℃ of lower calcining 6h, calcined material is taken out in cooling, and namely getting chemical formula after the grinding is Sr 2La 7.9(SiO 4) 6O 2: 0.01Tb 3+Silicate luminescent material.
Fig. 1 is that embodiment 1 makes silicate luminescent material and luminescent material (Zn 2SiO 4: luminescent spectrum comparison diagram Mn); Wherein, curve a represents luminescent material (Zn 2SiO 4: luminosity curve Mn); Curve b represents the luminosity curve figure of the silicate luminescent material that embodiment 1 makes.
Shown in Figure 1: under the 5kV electron-beam excitation, the Sr of present embodiment 1 preparation 2La 7.9(SiO 4) 6O 2: 0.01Tb 3+The luminous intensity of luminescent material (relative luminous intensity is 145) exceeds Zn 2SiO 4: the luminous intensity of Mn luminescent material (relative luminous intensity is 126) 15%.
Embodiment 2
Sr 2La 7.99(SiO 4) 6O 2:0.001Tm 3+
Take by weighing respectively the SrCO that total mass number is 2.9526g, 13.0161g, 3.6051g, 0.0020g 3, La 2O 3, SiO 2, Tm 2O 3Place agate mortar, after the grinding evenly, obtain mixed powder, then mixed powder is put into corundum crucible; Place air atmosphere lower corundum crucible, at 1600 ℃ of lower calcining 1h, cooling, taking-up namely gets Sr after grinding 2La 7.99(SiO 4) 6O 2: 0.001Tm 3+Silicate luminescent material.
Embodiment 3
Ca 2Y 7.5(SiO 4) 6O 2:0.5Tb 3+
Take by weighing respectively the CaCO that total mass number is 2.0016g, 13.4189g, 3.6051g, 0.9346g 3, Y 2(CO 3) 3, SiO 2, Tb 4O 7Place agate mortar, grind evenly after, obtain mixed powder, then mixed powder is put into corundum crucible, subsequently corundum crucible being placed volume ratio is 95: 5 N 2And H 2In the reducing atmosphere that forms, at 800 ℃ of lower calcining 10h, cooling, taking-up namely gets Ca after grinding 2Y 7.5(SiO 4) 6O 2: 0.5Tb 3+Silicate luminescent material.
Embodiment 4
Ca 1.5Sr 0.5La 7.8(SiO 4) 6O 2:0.2Dy 3+
Take by weighing respectively the SrCO that total mass number is 0.7381g, 1.5014g, 12.7065g, 4.6860g, 0.7460g 3, CaCO 3, La 2O 3, H 2SiO 3, Dy 2O 3Place agate mortar, after grinding is even, obtain mixed powder, then mixed powder is put into corundum crucible, place air atmosphere lower corundum crucible, at 1300 ℃ of lower calcining 4h, cool off, taking-up namely gets Ca after grinding 1.5Sr 0.5La 7.8(SiO 4) 6O 2: 0.2Dy 3+Silicate luminescent material.
Embodiment 5
Ca 1.5Mg 0.5Y 7.9(SiO 4) 6O 2:0.02Gd 3+，0.08Eu 3+
Take by weighing respectively the CaC that total mass number is 1.9215g, 0.4217g, 8.9195g, 4.6860g, 0.0363g, 0.2633g 2O 4, MgCO 3, Y 2O 3, H 2SiO 3, Gd 2O 3, Eu (O 2C 2H 3) 3 place agate mortar, grind evenly after, obtain mixed powder, then mixed powder is put into corundum crucible, place air atmosphere lower corundum crucible, at 1300 ℃ of lower calcining 5h, cooling namely gets Ca after taking out grinding 1.5Mg 0.5Y 7.9(SiO 4) 6O 2: 0.02Gd 3+, 0.08Eu 3+Silicate luminescent material.
Embodiment 6
Ba 2Y 0.9La 7(SiO 4) 6O 2:0.02Ce 3+，0.08Sm 3+
Take by weighing respectively the BaCO that total mass number is 3.9467g, 1.9884g, 11.4033g, 3.6051g, 0.0344g, 0.1395g 3, Y 2(C 2O 4) 3, La 2O 3, SiO 2, CeO 2, Sm 2O 3Place agate mortar, grind evenly after, obtain mixed powder, then mixed powder is put into corundum crucible, subsequently corundum crucible being placed volume ratio is 95: 5 N 2And H 2In the reducing atmosphere that forms, at 1000 ℃ of lower calcining 5h, cooling, taking-up namely gets Ba after grinding 2Y 0.9La 7(SiO 4) 6O 2: 0.02Ce 3+, 0.08Sm 3+Red illuminating material.
Should be understood that above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, scope of patent protection of the present invention should be as the criterion with claims.

Claims (7)

1. a silicate luminescent material is characterized in that, its chemical formula is:
M 2Ln 8-x(SiO 4) 6O 2: xRE 3+Wherein, M is one or both in Sr, Ba, Mg and the Ca element; Ln is at least a in Y and the La element; RE is one or both in Tb, Gd, Sm, Eu, Dy, Ce and the Tm element; X is stoichiometric coefficient, and the span of x is 0.001～0.5.
2. the preparation method of a silicate luminescent material is characterized in that, comprises the steps:
(1), according to chemical formula M 2Ln 8-x(SiO 4) 6O 2: xRE 3+In the stoichiometric ratio of each element, take by weighing the source compound of M, the source compound of Ln, the source compound of RE and the source compound of Si, grind, evenly mix, obtain mixed powder;
(2), in air atmosphere or reducing atmosphere, step (1) is obtained mixed powder at 800～1600 ℃ of lower insulation calcining 1～10h, then be cooled to room temperature, take out calcined material, namely get silicate luminescent material after the grinding, the chemical formula of this silicate luminescent material is M 2Ln 8-x(SiO 4) 6O 2: xRE 3+Wherein,
M is one or both in Sr, Ba, Mg and the Ca element; Ln is at least a in Y and the La element; RE is one or both in Tb, Gd, Sm, Eu, Dy, Ce and the m element; X is stoichiometric coefficient, and the span of x is 0.001～0.5.
3. the preparation method of silicate luminescent material according to claim 2 is characterized in that, in the step (1), the source compound of described M is selected from carbonate or the oxalate of M.
4. the preparation method of silicate luminescent material according to claim 2 is characterized in that, in the step (1), the source compound of described Ln is selected from oxide compound, acetate, carbonate or oxalate.
5. the preparation method of silicate luminescent material according to claim 2 is characterized in that, in the step (1), the source compound of described RE is selected from oxide compound, acetate, carbonate or oxalate.
6. the preparation method of silicate luminescent material according to claim 2 is characterized in that, in the step (1), the source compound of described Si is selected from SiO 2Or H 2SiO 3
7. the preparation method of silicate luminescent material according to claim 2 is characterized in that, in the step (2), described reducing atmosphere is that volume ratio is 95: 5 N 2And H 2Mixed atmosphere.
CN2012100882489A 2012-03-29 2012-03-29 Silicate luminous material and preparation method thereof Pending CN103361053A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107353902A (en) * 2017-07-31 2017-11-17 长安大学 Silicate fluorescent material for LED white lights and preparation method thereof
CN108998025A (en) * 2018-07-31 2018-12-14 景德镇陶瓷大学 A kind of LED silicate-base red fluorescence powder and preparation method thereof
CN112779009A (en) * 2021-02-05 2021-05-11 淮阴师范学院 High-sensitivity optical temperature sensing luminescent material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
于敏等: "《CaY8(SiO4)6O2：RE(RE=Eu，Tb)发光薄膜的制备及发光性能的研究》", 《中国稀土学报》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107353902A (en) * 2017-07-31 2017-11-17 长安大学 Silicate fluorescent material for LED white lights and preparation method thereof
CN108998025A (en) * 2018-07-31 2018-12-14 景德镇陶瓷大学 A kind of LED silicate-base red fluorescence powder and preparation method thereof
CN112779009A (en) * 2021-02-05 2021-05-11 淮阴师范学院 High-sensitivity optical temperature sensing luminescent material and preparation method thereof

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Application publication date: 20131023