CN1325604C - MY(1-x)SiO4:Ax light-emitting film and its preparation method - Google Patents

MY(1-x)SiO4:Ax light-emitting film and its preparation method Download PDF

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Publication number
CN1325604C
CN1325604C CNB2005101220368A CN200510122036A CN1325604C CN 1325604 C CN1325604 C CN 1325604C CN B2005101220368 A CNB2005101220368 A CN B2005101220368A CN 200510122036 A CN200510122036 A CN 200510122036A CN 1325604 C CN1325604 C CN 1325604C
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light
film
electron beam
emitting film
emitting
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CN1800302A (en
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李岚
张晓松
王达健
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Tianjin University of Technology
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Tianjin University of Technology
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Abstract

The present invention discloses a light-emitting film, the chemical expression of which is MY<1-x>SiO4: A<x>, wherein M is one of Na element and Li element, A is one element of Pr, Eu, Er, Tm, Ce, Lu, Nd and Sm, and x is larger than 0.001 and smaller than or equal to 0.5. The present invention is characterized in that raw materials adopt Na2CO3, Li2CO3, Y2O3, SiO2, Pr2O3, Eu2O3, Er2O3, Tm2O3, Ce2O3, Lu2O3, Nd2O3 and Sm2O3, the purity of which is 99.99 percent, and water and ethanol are used as solvent. The present invention also provides the preparation method for the light-emitting film. The light-emitting film prepared by the present invention has uniform and compact surfaces without cracks, uniform particles of the film, controllable thickness of the film and good light-emitting performance of the film. The light-emitting film of the present invention can be used for making a display screen of a field emission display, and the display screen not only can overcome the defects of the prior art, but also has the advantages of high thermal stability, low gas discharging rate, strong adhesive force, good surface smoothness, etc.

Description

MY (1-x)SiO 4: A xLight-emitting film and preparation method thereof
[technical field]
The present invention relates to luminous physical material and technique of display, particularly a kind of MY (1-x)SiO 4: A xLight-emitting film and preparation method thereof.
[background technology]
The display screen that luminescent material is made plays crucial effect in cathode tube, electroluminescent and field emission display.The display applications of at present luminescenjt powder being made exists many obstacles in Field Emission Display.Because the contact resistance between the particle, cause the specific conductivity of shielding not high.In addition, the sticking power problem between the particle and between particle and the substrate also is difficult to overcome.Simultaneously, the screen surfaces of this method preparation is coarse, and densification and lack of homogeneity cause reflection of light and stability bad easily, and resolving power is also lower.Therefore, the light-emitting film that processability is good becomes an important directions of research.
[summary of the invention]
The objective of the invention is in order to overcome the deficiencies in the prior art, and provide a kind of luminescent properties good MY (1-x)SiO 4: A xLight-emitting film, and its preparation method of this light-emitting film.
The present invention is prepared as and addresses the above problem the technical scheme that is adopted, and provides a kind of MY (1-x)SiO 4: A xLight-emitting film is characterized in that it is 99.99% Na that said raw material is selected purity for use 2CO 3, Li 2CO 3, Y 2O 3, SiO 2, Pr 2O 3, Eu 2O 3, Er 2O 3, Tm 2O 3, Ce 2O 3, Lu 2O 3, Nd 2O 3, Sm 2O 3, solvent is water and ethanol; Its chemical expression is:
MY (1-x)SiO 4:A x
Wherein, M is Na, and a kind of element among the Li, A are Pr, Eu, Er, Tm, Ce, Lu, Nd, a kind of element among the Sm, 0.001＜x≤0.5.
The present invention also provides a kind of MY (1-x)SiO 4: A xThe light-emitting film preparation method is characterized in that said preparation process is:
1) raw material is mixed according to stoichiometric ratio, and the adding solvent fully grinds, adopt solid state reaction, calcination 2 hours in the reducing atmosphere under 600-1000 ℃ of high temperature, obtain target material, target material is through press forming, sintering 2 hours in 600-800 ℃ of reducing atmosphere then, and making diameter is the electron beam evaporation target of 3mm;
2) adopt the electron beam evaporation deposition system, substrate surface is cleaned after mask hides, be loaded on the swivel mount, put into the reaction chamber of electron beam evaporation deposition system, the electron beam evaporation target is packed in the crucible; Reaction chamber vacuum tightness is extracted into 10 at least -5Torr, heated substrate then, making underlayer temperature is 100-400 ℃, determines vacuum tightness, underlayer temperature, opens the electron beam gun power supply, evaporates.
3) film of electron beam evaporation preparation is put into the temperature programming stove, be heated to 500-700 ℃ with the speed of 100 ℃/h, and kept 2-3 hour.
Even, the fine and close nothing cracking in the light-emitting film surface of the present invention's preparation; The film particles size is even, and the thickness of film can be controlled; The luminescent properties of film is good; Light-emitting film of the present invention can be used for the display screen of fabricating yard emission display, and this display screen not only can overcome the shortcoming of prior art, but also have that thermostability height, venting rate are little, strong adhesion, surface finish advantages of higher.
[embodiment]
Employed raw material among the present invention, selecting purity for use is 99.99% Na 2CO 3, Li 2CO 3, Y 2O 3, SiO 2, Pr 2O 3, Eu 2O 3, Er 2O 3, Tm 2O 3, Ce 2O 3, Lu 2O 3, Nd 2O 3, Sm 2O 3, solvent is water and ethanol.
Its chemical expression is:
MY (1-x)SiO 4:A x
Wherein, M is a kind of element among Na or the Li, and A is Pr, Eu, Er, Tm, Ce, Lu, a kind of element among Nd or the Sm, 0.001＜x≤0.5.
At this film MY (1-x)SiO 4: A xChemical expression in, the numerical value of x also can be following scope:
0.01＜x≤0.5。
Reasonable light-emitting film can be expressed as with following chemical expression:
(1)NaY 0.94SiO 4:Eu 0.06；
(2)LiY 0.95SiO 4:Tm 0.05。
In addition, the data that can also press in the tabulation at the specific embodiment of light-emitting film are determined:
M A X
1 Na Eu 0.1
2 Na Ce 0.06
3 Na Pr 0.03
4 Na Nd 0.35
5 Li Eu， 0.08
6 Li Er 0.01
7 Li Nd 0.3
8 Li Lu 0.04
The preparation of light-emitting film of the present invention:
With NaY 0.94SiO 4: Eu 0.06Be example, according to stoichiometric ratio, with Na 2CO 3, Y 2O 3, SiO 2, Eu 2O 3, waits and mix, and adding ethanol fully grinds, adopt solid state reaction, calcination 2 hours in the reducing atmosphere obtains target material under 900 ℃ of high temperature, target material is through press forming, sintering 2 hours in 700 ℃ of reducing atmospheres then, and making diameter is the electron beam evaporation target of 3mm.Adopt the electron beam evaporation deposition systems produce, select ito glass, substrate surface is cleaned after mask hides, be loaded on the swivel mount, put into the reaction chamber of electron beam evaporation deposition system, the electron beam evaporation target is packed in the crucible as substrate.Reaction chamber vacuum tightness is extracted into 10 -5Torr, heated substrate then, making underlayer temperature is 200 ℃, determines vacuum tightness, base reservoir temperature, opens the electron beam gun power supply, evaporates.The speed of growth is set at 5_/s, and the thickness of film is 200nm.The film of electron beam evaporation preparation is put into the temperature programming stove, be heated to 600 ℃ with the speed of 100 ℃/h, and kept 3 hours.Even, the fine and close nothing cracking in gained light-emitting film surface, the film particles size is even.
The substrate material of light-emitting film can also adopt silicon, sapphire or glass etc. except that adopting ito glass.
When electron beam evaporation prepared film, the preferred temperature of heated substrate was 200-300 ℃.

Claims (6)

1 one kinds of MY (1-x)SiO 4: A xLight-emitting film is characterized in that it is 99.99% Na that said raw material is selected purity for use 2CO 3, Li 2CO 3, Y 2O 3, SiO 2, Pr 2O 3, Eu 2O 3, Er 2O 3, Tm 2O 3, Ce 2O 3, Lu 2O 3, Nd 2O 3, Sm 2O 3, solvent is water or ethanol; The chemical expression of prepared light-emitting film is:
MY (1-x)SiO 4:A x
Wherein, M is a kind of element among Na or the Li; A is Pr, Eu, Er, Tm, Ce, Lu, a kind of element among Nd or the Sm;
0.001＜x≤0.5。
2 according to the described light-emitting film of claim 1, it is characterized in that said
0.01＜x≤0.5。
3 according to claim 1 or 2 described light-emitting films, it is characterized in that the chemical expression of said light-emitting film is:
NaY 0.94SiO 4:Eu 0.06。
4 according to claim 1 or 2 described light-emitting films, it is characterized in that the chemical expression of said light-emitting film is:
LiY 0.95SiO 4:Tm 0.05。
The preparation method of the light-emitting film of 5 one kinds of claims 1 is characterized in that said preparation process is:
1) raw material is mixed according to stoichiometric ratio, and the adding solvent fully grinds, adopt solid state reaction, calcination 2 hours in the reducing atmosphere under 600-1000 ℃ of high temperature, obtain target material, target material is through press forming, sintering 2 hours in 600-800 ℃ of reducing atmosphere then, and making diameter is the electron beam evaporation target of 3mm;
2) adopt the electron beam evaporation deposition system, substrate surface is cleaned after mask hides, be loaded on the swivel mount, put into the reaction chamber of electron beam evaporation deposition system, the electron beam evaporation target is packed in the crucible; Reaction chamber vacuum tightness is extracted into 10 at least -5Torr, heated substrate then, making underlayer temperature is 100-400 ℃, determines vacuum tightness, underlayer temperature, opens the electron beam gun power supply, evaporates;
3) film of electron beam evaporation preparation is put into the temperature programming stove, be heated to 500-700 ℃ with the speed of 100 ℃/h, and kept 2-3 hour.
6 according to the described preparation method of claim 5, it is characterized in that saidly when electron beam evaporation prepares film, and the temperature of heated substrate is 200-300 ℃.
CNB2005101220368A 2005-11-30 2005-11-30 MY(1-x)SiO4:Ax light-emitting film and its preparation method Expired - Fee Related CN1325604C (en)

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CN102234508A (en) * 2010-04-20 2011-11-09 中国科学院上海硅酸盐研究所 Rare-earth-doped lutetium borate radiation detection material, and preparation and application thereof
CN102796517B (en) * 2011-05-23 2015-02-04 海洋王照明科技股份有限公司 Nitrogenous magnesium silicate film, and preparation method and application thereof
CN102807859B (en) * 2011-05-30 2015-04-01 海洋王照明科技股份有限公司 Europium-doped chloride calcium magnesium silicate luminescent film, preparation method and applications thereof
WO2013143102A1 (en) 2012-03-29 2013-10-03 海洋王照明科技股份有限公司 Silicate luminescent materials doped with metal nano particles and preparation methods therefor
CN102719252B (en) * 2012-06-12 2014-02-26 北京工业大学 Up-and-down-conversion luminescent high-transmittance amorphous fluoride film and preparation method thereof
CN103275717A (en) * 2013-06-04 2013-09-04 中山大学 Rare earth light conversion fluorescent powder and preparation method thereof
CN115029001B (en) * 2022-05-27 2023-04-28 山东大学 Deep ultraviolet up-conversion luminescent film, deep ultraviolet light source, preparation method and application thereof

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CN1064301A (en) * 1991-12-28 1992-09-09 上海跃龙有色金属有限公司 High quality red fluorescent powder and manufacturing process thereof
JPH0762339A (en) * 1993-08-30 1995-03-07 Fuji Xerox Co Ltd Fluorescencer film and its making
US5543080A (en) * 1989-09-20 1996-08-06 Fujitsu Limited Method of forming an x-ray image using photostimulable phosphor
JP2000160155A (en) * 1998-09-24 2000-06-13 Konica Corp Rare-earth metal activated alkaline earth metal fluorohalide-based phosphorescent fluorescent substance, its moistureproof treatment, radiological image converting panel and production of phosphorescent fluorescent substance
CN1513943A (en) * 2003-07-02 2004-07-21 中国科学院上海硅酸盐研究所 Preparation method of nano-level yttrium oxide base luminous powder doped with rare earth
CN1580183A (en) * 2003-08-05 2005-02-16 北京大学 Rare earth activated Y2SiO5 fluorescent powder, and its preparing method and use

Patent Citations (6)

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Publication number Priority date Publication date Assignee Title
US5543080A (en) * 1989-09-20 1996-08-06 Fujitsu Limited Method of forming an x-ray image using photostimulable phosphor
CN1064301A (en) * 1991-12-28 1992-09-09 上海跃龙有色金属有限公司 High quality red fluorescent powder and manufacturing process thereof
JPH0762339A (en) * 1993-08-30 1995-03-07 Fuji Xerox Co Ltd Fluorescencer film and its making
JP2000160155A (en) * 1998-09-24 2000-06-13 Konica Corp Rare-earth metal activated alkaline earth metal fluorohalide-based phosphorescent fluorescent substance, its moistureproof treatment, radiological image converting panel and production of phosphorescent fluorescent substance
CN1513943A (en) * 2003-07-02 2004-07-21 中国科学院上海硅酸盐研究所 Preparation method of nano-level yttrium oxide base luminous powder doped with rare earth
CN1580183A (en) * 2003-08-05 2005-02-16 北京大学 Rare earth activated Y2SiO5 fluorescent powder, and its preparing method and use

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