CN104140818A - Cerium-doped ternary scandium silicate luminescence film, and making method and application thereof - Google Patents

Cerium-doped ternary scandium silicate luminescence film, and making method and application thereof Download PDF

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Publication number
CN104140818A
CN104140818A CN201310168982.0A CN201310168982A CN104140818A CN 104140818 A CN104140818 A CN 104140818A CN 201310168982 A CN201310168982 A CN 201310168982A CN 104140818 A CN104140818 A CN 104140818A
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China
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cerium
races
emitting film
substrate
doping
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周明杰
王平
陈吉星
钟铁涛
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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 CN201310168982.0A priority Critical patent/CN104140818A/en
Publication of CN104140818A publication Critical patent/CN104140818A/en
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Abstract

The chemical formula of a cerium-doped ternary scandium silicate luminescence film is Me3Sc2Si3O12:xCe3<+>, wherein x is not more than 0.05 and not less than 0.01, Me3Sc2Si3O12 is a matrix, the cerium element is an activation element, and Me is Al, Ga, In or Tl. In the electroluminescent spectrum (EL) of the cerium-doped ternary scandium silicate luminescence film, a very strong luminescence peak exists in a 620nm wavelength zone, and the luminescence film can be used in thin-film electroluminescence displays. The invention also provides a making method and an application of the cerium-doped ternary scandium silicate luminescence film.

Description

Cerium doping three races scandium silicate light-emitting film, preparation method and application thereof
[technical field]
The present invention relates to a kind of cerium doping three races scandium silicate light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof.
[background technology]
Thin-film electroluminescent displays (TFELD), due to its active illuminating, total solids, the advantage such as shock-resistant, reaction is fast, visual angle is large, Applicable temperature is wide, operation is simple, has caused and paid close attention to widely, and development rapidly.At present, research colour and extremely panchromatic TFELD, the luminous film of exploitation multiband, is the developing direction of this problem.But, can be applicable to the cerium doping three races scandium silicate light-emitting film of thin-film electroluminescent displays, have not yet to see report.
[summary of the invention]
Based on this, be necessary to provide a kind of cerium doping three races scandium silicate light-emitting film that can be applicable to membrane electro luminescent device, this cerium doping three races scandium silicate light-emitting film electroluminescent device of its preparation method and preparation method thereof.
One cerium doping three races scandium silicate light-emitting film, its chemical formula is Me 3sc 2si 3o 12: xCe 3+, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.
The thickness of cerium doping three races scandium silicate light-emitting film is 80nm～300nm.
A preparation method for cerium doping three races scandium silicate light-emitting film, comprises the following steps:
Substrate is packed in the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa～1.0 × 10 -3pa;
Regulating substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to Me 3sc 2si 3o 12: xCe 3+the stoichiometric ratio of each element passes into dipivaloylmethane alkaline earth salt, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium in reaction chamber, and
Then pass into oxygen, carrying out chemical vapour deposition, to obtain cerium doping three races its chemical formula of scandium silicate light-emitting film be Me 3sc 2si 3o 12: xCe 3+cerium doping three races scandium silicate light-emitting film, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.
Dipivaloylmethane alkaline earth salt, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium mol ratio are 3:2:3:(0.01～0.05);
Argon stream amount is 5～15sccm, and oxygen flow amount is 10～200sccm.
A kind of membrane electro luminescent device, this membrane electro luminescent device comprises the substrate, anode layer, luminescent layer and the cathode layer that stack gradually, the material of described luminescent layer is cerium doping three races scandium silicate light-emitting film, and the chemical formula of this cerium doping three races scandium silicate light-emitting film is Me 3sc 2si 3o 12: xCe 3+, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.
A preparation method for membrane electro luminescent device, comprises the following steps:
The substrate with anode is provided;
On described anode, form luminescent layer, the material of described luminescent layer is cerium doping three races scandium silicate light-emitting film, and the chemical formula of this cerium doping three races scandium silicate light-emitting film is Me 3sc 2si 3o 12: xCe 3+, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl;
On described luminescent layer, form negative electrode.
In a preferred embodiment, the preparation of described luminescent layer comprises the following steps:
Substrate is packed in the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa～1.0 × 10 -3pa;
Regulating substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to Me 3sc 2si 3o 12: xCe 3+the stoichiometric ratio of each element is by (DPM) 3me, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium pass in reaction chamber, and wherein, argon stream amount is 5～15sccm, and
Then pass into oxygen, flow is 10～200sccm; Carrying out chemical vapour deposition, to obtain luminescent layer chemical formula be Me 3sc 2si 3o 12: xCe 3+cerium doping three races scandium silicate light-emitting film, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.
The above-mentioned cerium doping scandium silicate light-emitting film (Me of three races 3sc 2si 3o 12: xCe 3+) electroluminescent spectrum (EL) in, have very strong glow peak in 620nm wavelength zone, can be applied in thin-film electroluminescent displays.
[brief description of the drawings]
Fig. 1 is the structural representation of the membrane electro luminescent device of an embodiment;
Fig. 2 is the electroluminescent spectrogram of the cerium doping three races scandium silicate light-emitting film prepared of embodiment 1;
Fig. 3 is the XRD figure of the cerium doping three races scandium silicate light-emitting film prepared of embodiment 1;
Fig. 4 is voltage and electric current and the brightness relationship figure of the membrane electro luminescent device prepared of embodiment 1.
[embodiment]
Below in conjunction with the drawings and specific embodiments, cerium doping three races scandium silicate light-emitting film, its preparation method and membrane electro luminescent device and preparation method thereof are further illustrated.
The cerium doping three races scandium silicate light-emitting film of one embodiment, its chemical formula is Me 3sc 2si 3o 12: xCe 3+, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.
Preferably, the thickness of cerium doping three races scandium silicate light-emitting film is 80nm～300nm, and x is 0.03.
Me in this cerium doping three races scandium silicate light-emitting film 3sc 2si 3o 12be matrix, Ce elements is active element.In the electroluminescent spectrum (EL) of this cerium doping three races scandium silicate light-emitting film, there is very strong glow peak in 620nm wavelength zone, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned cerium doping three races scandium silicate light-emitting film, comprises the following steps:
Step S11, substrate is packed in the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa～1.0 × 10 -3pa.
In the present embodiment, substrate is indium tin oxide glass (ITO), is appreciated that in other embodiments, also can be for fluorine doped tin oxide glass (FTO), mix the zinc oxide (AZO) of aluminium or mix the zinc oxide (IZO) of indium; Substrate is successively with toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into reaction chamber;
Preferably, the vacuum tightness of reaction chamber is 4.0 × 10 -3pa.
Step S12, by substrate thermal treatment 10 minutes～30 minutes at 600 DEG C～800 DEG C.
Step S13, adjusting substrate temperature are 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to Me 3sc 2si 3o 12: xCe 3+the stoichiometric ratio of each element is by (DPM) 3me, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium pass in reaction chamber;
Described dipivaloylmethane alkaline earth salt ((DPM) 3me), three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium mol ratio be 3:2:3:(0.01～0.05);
Described substrate temperature is preferably 500 DEG C, and the rotating speed of substrate is preferably 300 revs/min, and argon stream amount is 5～15sccm;
Described argon stream amount is 10sccm;
Step S14, then pass into oxygen, carrying out chemical vapour deposition, to obtain cerium doping three races its chemical formula of scandium silicate light-emitting film be Me 3sc 2si 3o 12: xCe 3+, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.
Described oxygen flow amount is 10～200sccm, and x is 0.03.
More preferably oxygen flow amount is 120sccm.
After step S15, deposition, stop passing into (DPM) 3me, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium and helium, continue to pass into oxygen and make the temperature of cerium doping three races scandium silicate light-emitting film be down to 80 DEG C～150 DEG C.
In present embodiment, preferred, make the temperature of cerium doping three races scandium silicate light-emitting film be down to 100 DEG C.
Be appreciated that step S12 and step S15 can omit.
Refer to Fig. 1, the membrane electro luminescent device 100 of an embodiment, this membrane electro luminescent device 100 comprises the substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 that stack gradually.
Substrate 1 is glass substrate.Anode 2 is for being formed at the tin indium oxide (ITO) in glass substrate.The material of luminescent layer 3 is cerium doping three races scandium silicate light-emitting film, and the chemical formula of this cerium doping three races scandium silicate light-emitting film is Me 3sc 2si 3o 12: xCe 3+, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.The material of negative electrode 4 is silver (Ag).
The preparation method of above-mentioned membrane electro luminescent device, comprises the following steps:
Step S21, provide the substrate 1 with anode 2.
In present embodiment, substrate 1 is glass substrate, and anode 2 is for being formed at the tin indium oxide (ITO) in glass substrate.Be appreciated that in other embodiments, also can be for fluorine doped tin oxide glass (FTO), mix the zinc oxide (AZO) of aluminium or mix the zinc oxide (IZO) of indium; The substrate 1 with anode 2 is successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning and use it is carried out to oxygen plasma treatment.
Step S22, on anode 2, form luminescent layer 3, the material of luminescent layer 3 is cerium doping three races scandium silicate light-emitting film, and the chemical formula of this cerium doping three races scandium silicate light-emitting film is Me 3sc 2si 3o 12: xCe 3+, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.
In present embodiment, luminescent layer 3 is made by following steps:
First, substrate is packed in the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa～1.0 × 10 -3pa;
Moreover, by substrate thermal treatment 10 minutes～30 minutes at 600 DEG C～800 DEG C.Also can be without this step.
Secondly, regulating substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to Me 3sc 2si 3o 12: xCe 3+the stoichiometric ratio of each element is by (DPM) 3me, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium pass in reaction chamber;
In a preferred embodiment, (DPM) 3me, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium mol ratio are 3:2:3:(0.01～0.05);
In a preferred embodiment, substrate temperature is preferably 500 DEG C, and the rotating speed of substrate is preferably 300 revs/min, and argon stream amount is 5～15sccm;
In more preferred embodiment, argon stream amount is 10sccm;
Then pass into oxygen, carry out chemical vapour deposition film and form luminescent layer on described anode.
In preferred embodiment, the flow of oxygen is preferably 10～200sccm;
In more preferred embodiment, oxygen flow amount is 120sccm.
Finally, after deposition, stop passing into (DPM) 3me, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium and helium, continue to pass into oxygen and make the temperature of cerium doping three races scandium silicate light-emitting film be down to 80 DEG C～150 DEG C.
In present embodiment, preferred, make the temperature of cerium doping three races scandium silicate light-emitting film be down to 100 DEG C.Can be without this step.
Step S23, on luminescent layer 3, form negative electrode 4.
In present embodiment, the material of negative electrode 4 is silver (Ag), is formed by evaporation.
Be specific embodiment below.
Embodiment 1
Substrate is ito glass, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 4.0 × 10 with mechanical pump and molecular pump -3pa; Then substrate is carried out to 700 DEG C of thermal treatments 20 minutes, then temperature is reduced to 500 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 300 revs/min, passes into organic source (DPM) 3al, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.03, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample Al 3sc 2si 3o 12: 0.03Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the cerium doping three races scandium silicate light-emitting film obtaining in the present embodiment is Al 3sc 2si 3o 12: 0.03Ce 3+, wherein Al 3sc 2si 3o 12be matrix, Ce elements is active element.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the cerium doping three races scandium silicate light-emitting film that embodiment 1 obtains.The electroluminescent spectral curve of the cerium doping three races scandium silicate light-emitting film that as seen from Figure 2, embodiment 1 obtains has very strong glow peak can be applied in thin-film electroluminescent displays in 620nm wavelength zone.
Refer to Fig. 3, Fig. 3 is the XRD curve of the cerium doping three races scandium silicate light-emitting film prepared of embodiment 1, test comparison standard P DF card.As can be seen from Figure 3, reference standard PDF card, in figure, diffraction peak is depicted as the peak crystallization of three races's scandium silicate, does not occur the diffraction peak of doped element and other impurity, illustrates that the product that this preparation method obtains has good crystalline quality.
Refer to Fig. 4, Fig. 4 is voltage and electric current and the brightness relationship figure of the membrane electro luminescent device prepared of embodiment 1, and curve 1 is voltage-to-current density, can find out that device starts from 5.0V luminous, and curve 2 is voltage-brightness, and high-high brightness is 86cd/m 2, show that device has the good characteristics of luminescence.
Embodiment 2
Substrate is ito glass, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump -3pa; Then substrate is carried out to 700 DEG C of thermal treatments 10 minutes, then temperature is reduced to 250 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 50 revs/min, passes into machine source (DPM) 3al, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.06, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample Al 3sc 2si 3o 12: 0.06Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 3
Substrate is ito glass, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump -2pa; Then substrate is carried out to 700 DEG C of thermal treatments 30 minutes, then temperature is reduced to 650 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 1000 revs/min, passes into organic source (DPM) 3al, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.01, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample Al 3sc 2si 3o 12: 0.01Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 4: substrate is ito glass, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 4.0 × 10 with mechanical pump and molecular pump -3pa; Then substrate is carried out to 700 DEG C of thermal treatments 20 minutes, then temperature is reduced to 500 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 300 revs/min, passes into organic source (DPM) 3ga, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.03, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample Ga 3sc 2si 3o 12: 0.03Ce 3+finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 5: substrate is the ito glass that Nan Bo company buys, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump -3pa; Then substrate is carried out to 700 DEG C of thermal treatments 10 minutes, then temperature is reduced to 250 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 50 revs/min, passes into machine source (DPM) 3ga, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.06, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample Ga 3sc 2si 3o 12: 0.06Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 6: substrate is the ito glass that Nan Bo company buys, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump -2pa; Then substrate is carried out to 700 DEG C of thermal treatments 30 minutes, then temperature is reduced to 650 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 1000 revs/min, passes into organic source dicyclopentadiene calcium (DPM) 3ga, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.01, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample Ga 3sc 2si 3o 12: 0.01Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 7: substrate is the ito glass that Nan Bo company buys, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 4.0 × 10 with mechanical pump and molecular pump -3pa; Then substrate is carried out to 700 DEG C of thermal treatments 20 minutes, then temperature is reduced to 500 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 300 revs/min, passes into organic source (DPM) 3in, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.03, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample In 3sc 2si 3o 12: 0.03Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 8: substrate is the ito glass that Nan Bo company buys, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump -3pa; Then substrate is carried out to 700 DEG C of thermal treatments 10 minutes, then temperature is reduced to 250 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 50 revs/min, passes into organic source (DPM) 3in, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.06, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample In 3sc 2si 3o 12: 0.06Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 9: substrate is the ito glass that Nan Bo company buys, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump -2pa; Then substrate is carried out to 700 DEG C of thermal treatments 30 minutes, then temperature is reduced to 650 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 1000 revs/min, passes into machine source (DPM) 3in, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.01, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample In 3sc 2si 3o 12: 0.01Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 10: substrate is the ito glass that Nan Bo company buys, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 4.0 × 10 with mechanical pump and molecular pump -3pa; Then substrate is carried out to 700 DEG C of thermal treatments 20 minutes, then temperature is reduced to 500 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 300 revs/min, passes into machine source (DPM) 3tl, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.03, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample Tl 3sc 2si 3o 12: 0.03Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 11: substrate is the ito glass that Nan Bo company buys, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump -3pa; Then substrate is carried out to 700 DEG C of thermal treatments 10 minutes, then temperature is reduced to 250 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 50 revs/min, passes into machine source (DPM) 3tl, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.06, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample Tl 3sc 2si 3o 12: 0.06Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 12: substrate is the ito glass that Nan Bo company buys, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump -2pa; Then substrate is carried out to 700 DEG C of thermal treatments 30 minutes, then temperature is reduced to 650 DEG C.Open rotating machine, regulating the rotating speed of substrate bracket is 1000 revs/min, passes into machine source (DPM) 3tl, three carbonyl scandiums (Sc (CO) 3), silane (SiH 4) and the mol ratio of four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium be 3:2:3:0.01, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 DEG C, takes out sample Tl 3sc 2si 3o 12: 0.01Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (10)

1. a cerium doping three races scandium silicate light-emitting film, is characterized in that, its chemical formula is Me 3sc 2si 3o 12: xCe 3+, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.
2. cerium according to claim 1 doping three races scandium silicate light-emitting film, is characterized in that, the thickness of described cerium doping three races scandium silicate light-emitting film is 80nm～300nm.
3. a preparation method for cerium doping three races scandium silicate light-emitting film, is characterized in that, comprises the following steps:
Substrate is packed in the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa～1.0 × 10 -3pa;
Regulating substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to Me 3sc 2si 3o 12: xCe 3+the stoichiometric ratio of each element passes into dipivaloylmethane alkaline earth salt, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium in reaction chamber; And
Pass into oxygen, carrying out chemical vapour deposition, to obtain chemical formula be Me 3sc 2si 3o 12: xCe 3+cerium doping three races scandium silicate light-emitting film, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.
4. the preparation method of cerium according to claim 3 doping three races scandium silicate light-emitting film, it is characterized in that, described dipivaloylmethane alkaline earth salt, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3,5-heptadione acid) cerium mol ratio is 3:2:3:(0.01～0.05).
5. the preparation method of cerium according to claim 3 doping three races scandium silicate light-emitting film, is characterized in that, described argon stream amount is 5～15sccm, and described oxygen flow amount is 10～200sccm.
6. the preparation method of cerium according to claim 3 doping three races scandium silicate light-emitting film, is characterized in that, described substrate is packed into after described reaction chamber the thermal treatment 10 minutes～30 minutes at 600 DEG C～800 DEG C of described substrate.
7. a membrane electro luminescent device, this membrane electro luminescent device comprises the substrate, anode layer, luminescent layer and the cathode layer that stack gradually, it is characterized in that, the material of described luminescent layer is cerium doping three races scandium silicate light-emitting film, and the chemical formula of this cerium doping three races scandium silicate light-emitting film is Me 3sc 2si 3o 12: xCe 3+, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl.
8. membrane electro luminescent device according to claim 7, is characterized in that, the thickness of described luminescent layer is 80nm～300nm.
9. a preparation method for membrane electro luminescent device, is characterized in that, comprises the following steps:
The substrate with anode is provided;
On described anode, form luminescent layer, the film of described luminescent layer is cerium doping three races scandium silicate light-emitting film, and the chemical formula of this cerium doping three races scandium silicate light-emitting film is Me 3sc 2si 3o 12: xCe 3+, wherein, 0.01≤x≤0.05, Me 3sc 2si 3o 12be matrix, Ce elements is active element, and Me is Al, Ga, In or Tl;
On described luminescent layer, form negative electrode.
10. the preparation method of membrane electro luminescent device according to claim 9, is characterized in that, the preparation of described luminescent layer comprises the following steps:
Described substrate is packed into the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa～1.0 × 10 -3pa;
Regulating substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts argon stream as carrier, according to Me 3sc 2si 3o 12: xCe 3+the stoichiometric ratio of each element passes into dipivaloylmethane alkaline earth salt, three carbonyl scandiums, silane and four (2,2,6,6-tetramethyl--3, the acid of 5-heptadione) cerium in reaction chamber, and wherein, argon stream amount is 5～15sccm;
Then pass into oxygen, oxygen flow amount is 10～200sccm; Deposit film forms luminescent layer on described anode.
CN201310168982.0A 2013-05-06 2013-05-06 Cerium-doped ternary scandium silicate luminescence film, and making method and application thereof Pending CN104140818A (en)

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Citations (3)

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Publication number Priority date Publication date Assignee Title
JPH0837328A (en) * 1994-07-25 1996-02-06 Nippon Telegr & Teleph Corp <Ntt> Garnet crystal waveguide for tunable laser
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Publication number Priority date Publication date Assignee Title
JPH0837328A (en) * 1994-07-25 1996-02-06 Nippon Telegr & Teleph Corp <Ntt> Garnet crystal waveguide for tunable laser
CN101263213A (en) * 2005-09-15 2008-09-10 住友化学株式会社 Fluorescent substance
WO2009083852A2 (en) * 2007-12-21 2009-07-09 Koninklijke Philips Electronics N.V. Radiation-sensitive detector with a scintillator in a composite resin

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Application publication date: 20141112