CN1775998A - MGd(1x)SiO4:Ax luminous film and preparing method - Google Patents

MGd(1x)SiO4:Ax luminous film and preparing method Download PDF

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Publication number
CN1775998A
CN1775998A CN 200510122038 CN200510122038A CN1775998A CN 1775998 A CN1775998 A CN 1775998A CN 200510122038 CN200510122038 CN 200510122038 CN 200510122038 A CN200510122038 A CN 200510122038A CN 1775998 A CN1775998 A CN 1775998A
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China
Prior art keywords
electron beam
light
sio
film
beam evaporation
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CN 200510122038
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Chinese (zh)
Inventor
张晓松
李岚
王达健
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Tianjin University of Technology
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Tianjin University of Technology
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Priority to CN 200510122038 priority Critical patent/CN1775998A/en
Publication of CN1775998A publication Critical patent/CN1775998A/en
Pending legal-status Critical Current

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  • Luminescent Compositions (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention relates to emitting film and the method to manufacture. The feature is that it adopts Na2CO3, LiCO3, Gd2O3, SiO2, Pr2O3, Eu2O3, Er2O3, Tm2O3, Ce2O3, Lu2O3, Nd2O3, Sm2O3 that the purity is 99.99% as raw material, and the solvent is water and alcohol. The invention has equal emitting film surface, compacting and no crazing, the particle is equal and the thickness could be controlled. The film has good emitting capability.

Description

MGd (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 MGd (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 MGd (1-x)SiO 4: A xLight-emitting film, and its preparation method of this light-emitting film.
The present invention addresses the above problem the technical scheme that is adopted, and provides a kind of MGd (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, Gd 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:
MGd (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.
The present invention also provides a kind of MGd (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, Gd 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:
MGd (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.
At this film MGd (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)NaGd 0.95SiO 4:Eu 0.05；
(2)LiGd 0.94SiO 4:Tm 0.06。
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 0.07
3 Na Pr 0.05
4 Na Tm 0.05
5 Na Lu 0.03
6 Li Eu 0.06
7 Li Er 0.02
8 Li Pr 0.3
The preparation of light-emitting film of the present invention:
With NaGd 0.94SiO 4: Eu 0.06Be example, according to stoichiometric ratio, with Na 2CO 3, Gd 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 temperature 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 MGd (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, Gd 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; The chemical expression of prepared light-emitting film is:
MGd (1-x)SiO 4:A x
Wherein, M is a kind of element among Na or the Li, and A is Pr, Eu, and 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 reasonable light-emitting film is:
NaGd 0.95SiO 4:Eu 0.05。
4 according to claim 1 or 2 described light-emitting films, it is characterized in that the chemical expression of said reasonable light-emitting film is:
LiGd 0.94SiO 4:Tm 0.06。
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 preferred temperature of heated substrate is 200-300 ℃.
CN 200510122038 2005-11-30 2005-11-30 MGd(1x)SiO4:Ax luminous film and preparing method Pending CN1775998A (en)

Priority Applications (1)

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CN 200510122038 CN1775998A (en) 2005-11-30 2005-11-30 MGd(1x)SiO4:Ax luminous film and preparing method

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Application Number Priority Date Filing Date Title
CN 200510122038 CN1775998A (en) 2005-11-30 2005-11-30 MGd(1x)SiO4:Ax luminous film and preparing method

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CN1775998A true CN1775998A (en) 2006-05-24

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102807859A (en) * 2011-05-30 2012-12-05 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
CN103275717A (en) * 2013-06-04 2013-09-04 中山大学 Rare earth light conversion fluorescent powder and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102807859A (en) * 2011-05-30 2012-12-05 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
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
CN103275717A (en) * 2013-06-04 2013-09-04 中山大学 Rare earth light conversion fluorescent powder and preparation method thereof

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