CN104342157A - Alkali metal and titanium ion co-doped strontium selenide luminescent thin film, and preparation method and application thereof - Google Patents

Alkali metal and titanium ion co-doped strontium selenide luminescent thin film, and preparation method and application thereof Download PDF

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Publication number
CN104342157A
CN104342157A CN201310336806.3A CN201310336806A CN104342157A CN 104342157 A CN104342157 A CN 104342157A CN 201310336806 A CN201310336806 A CN 201310336806A CN 104342157 A CN104342157 A CN 104342157A
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basic metal
selenizing
titanium
strontium
srse
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周明杰
陈吉星
王平
冯小明
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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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Abstract

The invention discloses an alkali metal and titanium ion co-doped strontium selenide luminescent thin film with a chemical formula of SrSe:xTi<4+>, yR<+>, wherein x is no lower than 0.01 and no higher than 0.08, y is no lower than 0 and no higher than 0.06, SrSe is a substrate, alkali metal and titanium element are activate elements, and R is lithium element, sodium element or potassium element. In an electro-luminescence spectrum (EL) of the alkali metal and titanium ion co-doped strontium selenide luminescent thin film, strong luminescence peak can be found at 410nm wavelength zone. The thin film can be used in an thin-film electroluminescent display device. The invention also provides a preparation method and an application of the alkali metal and titanium ion co-doped strontium selenide luminescent film.

Description

Basic metal and titanium ion codoped selenizing strontium light-emitting film, preparation method and application thereof
[technical field]
The present invention relates to a kind of basic metal and titanium ion codoped selenizing strontium 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 film of exploitation multiband luminescence is the developing direction of this problem.But, can be applicable to basic metal and the titanium ion codoped selenizing strontium 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 can be applicable to membrane electro luminescent device basic metal and titanium ion codoped selenizing strontium light-emitting film, this basic metal of its preparation method and titanium ion codoped selenizing strontium light-emitting film electroluminescent device and preparation method thereof.
A kind of basic metal and titanium ion codoped selenizing strontium light-emitting film, its chemical formula is SrSe:xTi 4+, yR +, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.
The thickness of basic metal and titanium ion codoped selenizing strontium light-emitting film is 80nm ~ 300nm.
A preparation method for basic metal and titanium ion codoped selenizing strontium light-emitting film, comprises the following steps:
Substrate is loaded 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;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, adopts the carrier of argon stream, according to SrSe:xTi 4+, yR +alkali metal source, dimethyl strontium source and titanium tetraisopropylate pass in reaction chamber by the stoichiometric ratio of each element, and
Then pass into Selenium hydride, carry out chemical vapour deposition and obtain basic metal and its chemical formula of titanium ion codoped selenizing strontium light-emitting film is SrSe:xTi 4+, yR +basic metal and titanium ion codoped selenizing strontium light-emitting film, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.
Dimethyl strontium source, titanium tetraisopropylate and alkali metal source mol ratio are (0.86 ~ 0.98): (0.01 ~ 0.08): (0.01 ~ 0.06);
Argon stream amount is 5 ~ 15sccm, and Selenium hydride airshed 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 basic metal and titanium ion codoped selenizing strontium light-emitting film, and the chemical formula of this basic metal and titanium ion codoped selenizing strontium light-emitting film is SrSe:xTi 4+, yR +, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.
A preparation method for membrane electro luminescent device, comprises the following steps:
The substrate with anode is provided;
Described anode forms luminescent layer, and the material of described luminescent layer is basic metal and titanium ion codoped selenizing strontium light-emitting film, and the chemical formula of this basic metal and titanium ion codoped selenizing strontium light-emitting film is SrSe:xTi 4+, yR +, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element;
Form negative electrode on the light-emitting layer.
In a preferred embodiment, the preparation of described luminescent layer comprises the following steps:
Substrate is loaded 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;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, adopts the carrier of argon stream, according to SrSe:xTi 4+, yR +alkali metal source, dimethyl strontium source and titanium tetraisopropylate pass in reaction chamber by the stoichiometric ratio of each element, and wherein, argon stream amount is 5 ~ 15sccm, and
Then pass into Selenium hydride, flow is 10 ~ 200sccm; Carrying out chemical vapour deposition, to obtain luminescent layer chemical formula be SrSe:xTi 4+, yR +basic metal and titanium ion codoped selenizing strontium light-emitting film, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.
Above-mentioned basic metal and titanium ion codoped selenizing strontium light-emitting film (SrSe:xTi 4+, yR +) electroluminescent spectrum (EL) in, have very strong glow peak in 410nm wavelength zone, can be applied in thin-film electroluminescent displays.
[accompanying drawing explanation]
Fig. 1 is the structural representation of the membrane electro luminescent device of an embodiment;
Fig. 2 is the basic metal of embodiment 1 preparation and the electroluminescent spectrogram of titanium ion codoped selenizing strontium light-emitting film;
Fig. 3 is the basic metal of embodiment 1 preparation and the XRD figure of titanium ion codoped selenizing strontium light-emitting film;
Fig. 4 is the voltage of membrane electro luminescent device prepared of embodiment 1 and electric current and brightness relationship figure.
[embodiment]
Below in conjunction with the drawings and specific embodiments, basic metal and titanium ion codoped selenizing strontium light-emitting film, its preparation method and membrane electro luminescent device and preparation method thereof are illustrated further.
The basic metal of one embodiment and titanium ion codoped selenizing strontium light-emitting film, its chemical formula is SrSe:xTi 4+, yR +, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.
Preferably, the thickness of basic metal and titanium ion codoped selenizing strontium light-emitting film is 80nm ~ 300nm, x be 0.05, y is 0.03.
In this basic metal and titanium ion codoped selenizing strontium light-emitting film, SrSe is matrix, and basic metal and titanium elements are active elements.In the electroluminescent spectrum (EL) of this basic metal and titanium ion codoped selenizing strontium light-emitting film, there is very strong glow peak in 410nm wavelength zone, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned basic metal and titanium ion codoped selenizing strontium light-emitting film, comprises the following steps:
Step S11, substrate to be loaded 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, can be also fluorine doped tin oxide glass (FTO), mixes the zinc oxide (AZO) of aluminium or mix the zinc oxide (IZO) of indium; Substrate priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, the air-dry rear feeding reaction chamber of nitrogen;
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, adjustment 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 SrSe:xTi 4+, yR +alkali metal source, dimethyl strontium source and titanium tetraisopropylate pass in reaction chamber by the stoichiometric ratio of each element;
In a preferred embodiment, dimethyl strontium source, titanium tetraisopropylate and alkali metal source mol ratio are (0.86 ~ 0.98): (0.01 ~ 0.08): (0.01 ~ 0.06);
Described alkali metal source comprises: ethylene glycol lithium, ethylene glycol sodium or ethylene glycol potassium;
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;
Step S14, then pass into Selenium hydride, carry out chemical vapour deposition and obtain basic metal and its chemical formula of titanium ion codoped selenizing strontium light-emitting film is SrSe:xTi 4+, yR +, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.
In a preferred embodiment, Selenium hydride airshed is 10 ~ 200sccm, x be 0.05, y is 0.03.
In more preferred embodiment, Selenium hydride airshed is 120sccm.
Stop passing into alkali metal source, dimethyl strontium source and titanium tetraisopropylate and helium after step S15, deposition, continue to pass into Selenium hydride and make the temperature of basic metal and titanium ion codoped selenizing strontium light-emitting film be down to 80 DEG C ~ 150 DEG C.
In present embodiment, preferably, the temperature of basic metal and titanium ion codoped selenizing strontium light-emitting film is made to 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 basic metal and titanium ion codoped selenizing strontium light-emitting film, and the chemical formula of this basic metal and titanium ion codoped selenizing strontium light-emitting film is SrSe:xTi 4+, yR +, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.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, can be also fluorine doped tin oxide glass (FTO), mix the zinc oxide (AZO) of aluminium or mix the zinc oxide (IZO) of indium; There is the substrate 1 priority acetone of anode 2, dehydrated alcohol and deionized water ultrasonic cleaning and carry out oxygen plasma treatment with to it.
Step S22, on anode 2, form luminescent layer 3, the material of luminescent layer 3 is basic metal and titanium ion codoped selenizing strontium light-emitting film, and the chemical formula of this basic metal and titanium ion codoped selenizing strontium light-emitting film is SrSe:xTi 4+, yR +, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.
In present embodiment, luminescent layer 3 is obtained by following steps:
First, substrate is loaded 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 without the need to this step.
Secondly, regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, adopts the carrier of argon stream, according to SrSe:xTi 4+, yR +alkali metal source, dimethyl strontium source and titanium tetraisopropylate pass in reaction chamber by the stoichiometric ratio of each element;
In a preferred embodiment, dimethyl strontium source, titanium tetraisopropylate and alkali metal source mol ratio are (0.86 ~ 0.98): (0.01 ~ 0.08): (0.01 ~ 0.06);
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 Selenium hydride, carry out chemical vapour deposition film and form luminescent layer on described anode.
In preferred embodiment, the flow of Selenium hydride is preferably 10 ~ 200sccm;
In more preferred embodiment, Selenium hydride airshed is 120sccm.
Finally, deposition after stop pass into alkali metal source, dimethyl strontium source and titanium tetraisopropylate and helium, continue to pass into Selenium hydride and make the temperature of basic metal and titanium ion codoped selenizing strontium light-emitting film be down to 80 DEG C ~ 150 DEG C.
In present embodiment, preferably, the temperature of basic metal and titanium ion codoped selenizing strontium light-emitting film is made to be down to 100 DEG C.Can without the need to 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 cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, and the mol ratio passing into organic source dimethyl strontium, titanium tetraisopropylate and ethylene glycol lithium is 1:0.05:0.03, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into Selenium hydride, Selenium hydride airshed is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical Selenium hydride, temperature drops to less than 100 DEG C, takes out sample SrSe:0.05Ti 4+, 0.03Li +.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the basic metal obtained in the present embodiment and titanium ion codoped selenizing strontium light-emitting film is SrSe:0.05Ti 4+, 0.03Li +, wherein SrSe is matrix, and elemental lithium and titanium elements are active elements.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the basic metal that embodiment 1 obtains and titanium ion codoped selenizing strontium light-emitting film.As seen from Figure 2, curve 1 is that the electroluminescent spectral curve of the basic metal that obtains of embodiment 1 and titanium ion codoped selenizing strontium light-emitting film has very strong glow peak can be applied in thin-film electroluminescent displays in 410nm wavelength zone, curve 2 is the metal co-doped comparative example of alkali-free, and its chemical formula is SrSe:0.05Ti 4+, obviously find out, with the addition of the codoped of alkalimetal ion, sample obtains higher luminous efficiency.
Refer to Fig. 3, Fig. 3 is the basic metal of embodiment 1 preparation and the XRD curve of titanium ion codoped selenizing strontium light-emitting film, test comparison standard P DF card.As can be seen from Figure 3, reference standard PDF card, can find out in figure X-ray diffraction peak corresponding be the characteristic peak of selenizing strontium, there is not doped element and the relevant peak of impurity, illustrate that dopant ion enters the lattice of selenizing strontium, sample has good crystallographic property.。
Refer to Fig. 4, Fig. 4 is the voltage of membrane electro luminescent device prepared of embodiment 1 and electric current and brightness relationship figure, and curve 1 is voltage-current density, and can find out device luminescence from 5.5V, curve 2 is voltage-brightness, and high-high brightness is 320cd/m 2, show that device has the good characteristics of luminescence.
Embodiment 2
Substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, and the mol ratio passing into machine source dimethyl strontium, titanium tetraisopropylate and ethylene glycol lithium is 1:0.08:0.06, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into Selenium hydride, Selenium hydride airshed is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical Selenium hydride, temperature drops to less than 100 DEG C, takes out sample SrSe:0.08Ti 4+, 0.06Li +.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 3
Substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, and the mol ratio passing into organic source dimethyl strontium and titanium tetraisopropylate is 1:0.01, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into Selenium hydride, Selenium hydride airshed is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical Selenium hydride, temperature drops to less than 100 DEG C, takes out sample SrSe:0.01Ti 4+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 4: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, and the mol ratio passing into organic source dimethyl strontium, titanium tetraisopropylate and ethylene glycol sodium is 1:0.05:0.03, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into Selenium hydride, Selenium hydride airshed is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical Selenium hydride, temperature drops to less than 100 DEG C, takes out sample SrSe:0.05Ti 4+, 0.03Na +finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 5: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, and the mol ratio passing into machine source dimethyl strontium, titanium tetraisopropylate and ethylene glycol sodium is 1:0.08:0.06, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into Selenium hydride, Selenium hydride airshed is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical Selenium hydride, temperature drops to less than 100 DEG C, takes out sample SrSe:0.08Ti 4+, 0.06Na +.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 6: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, and the mol ratio passing into organic source dimethyl strontium, titanium tetraisopropylate and ethylene glycol potassium is 1:0.05:0.03, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into Selenium hydride, Selenium hydride airshed is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical Selenium hydride, temperature drops to less than 100 DEG C, takes out sample SrSe:0.05Ti 4+, 0.03K +.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 7: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, and the mol ratio passing into organic source dimethyl strontium, titanium tetraisopropylate and ethylene glycol potassium is 1:0.08:0.06, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into Selenium hydride, Selenium hydride airshed is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical Selenium hydride, temperature drops to less than 100 DEG C, takes out sample SrSe:0.08Ti 4+, 0.06K +.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 8: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, and the mol ratio passing into organic source dimethyl strontium, titanium tetraisopropylate and ethylene glycol potassium is 1:0.0.4:0.0.4, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into Selenium hydride, Selenium hydride airshed is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical Selenium hydride, temperature drops to less than 100 DEG C, takes out sample SrSe:0.04Ti 4+, 0.04K +.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 9: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, and the mol ratio passing into machine source dimethyl strontium, titanium tetraisopropylate and ethylene glycol sodium is 1:0.03:0.03, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into Selenium hydride, Selenium hydride airshed is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical Selenium hydride, temperature drops to less than 100 DEG C, takes out sample SrSe:0.03Ti 4+, 0.03Na +.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 10: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, and the mol ratio passing into machine source dimethyl strontium, titanium tetraisopropylate and ethylene glycol lithium is 1:0.02:0.04, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into Selenium hydride, Selenium hydride airshed is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical Selenium hydride, temperature drops to less than 100 DEG C, takes out sample SrSe:0.02Ti 4+, 0.04Li +.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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. basic metal and a titanium ion codoped selenizing strontium light-emitting film, it is characterized in that, its chemical formula is SrSe:xTi 4+, yR +, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.
2. basic metal according to claim 1 and titanium ion codoped selenizing strontium light-emitting film, is characterized in that, the thickness of described basic metal and titanium ion codoped selenizing strontium light-emitting film is 80nm ~ 300nm.
3. a preparation method for basic metal and titanium ion codoped selenizing strontium light-emitting film, is characterized in that, comprise the following steps:
Substrate is loaded 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;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, adopts the carrier of argon stream, according to SrSe:xTi 4+, yR +alkali metal source, dimethyl strontium source and titanium tetraisopropylate pass in reaction chamber by the stoichiometric ratio of each element; And
Pass into Selenium hydride, carrying out chemical vapour deposition, to obtain chemical formula be SrSe:xTi 4+, yR +basic metal and titanium ion codoped selenizing strontium light-emitting film, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.
4. the preparation method of basic metal according to claim 3 and titanium ion codoped selenizing strontium light-emitting film, it is characterized in that, described dimethyl strontium source, titanium tetraisopropylate and alkali metal source mol ratio are (0.86 ~ 0.98): (0.01 ~ 0.08): (0.01 ~ 0.06).
5. the preparation method of basic metal according to claim 3 and titanium ion codoped selenizing strontium light-emitting film, it is characterized in that, described argon stream amount is 5 ~ 15sccm, and described Selenium hydride airshed is 10 ~ 200sccm.
6. the preparation method of basic metal according to claim 3 and titanium ion codoped selenizing strontium light-emitting film, is characterized in that, is loaded the thermal treatment 10 minutes ~ 30 minutes at 600 DEG C ~ 800 DEG C of described substrate by described substrate after described reaction chamber.
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 basic metal and titanium ion codoped selenizing strontium light-emitting film, and the chemical formula of this basic metal and titanium ion codoped selenizing strontium light-emitting film is SrSe:xTi 4+, yR +, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element.
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;
Described anode forms luminescent layer, and the film of described luminescent layer is basic metal and titanium ion codoped selenizing strontium light-emitting film, and the chemical formula of this basic metal and titanium ion codoped selenizing strontium light-emitting film is SrSe:xTi 4+, yR +, wherein, 0.01≤x≤0.08,0≤y≤0.06, SrSe is matrix, and basic metal and titanium elements are active elements, and R is elemental lithium, sodium element or potassium element;
Form negative electrode on the light-emitting layer.
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 loaded 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;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, adopts argon stream as carrier, according to SrSe:xTi 4+, yR +alkali metal source, dimethyl strontium source and titanium tetraisopropylate pass in reaction chamber by the stoichiometric ratio of each element, and wherein, argon stream amount is 5 ~ 15sccm,
Then pass into Selenium hydride, Selenium hydride airshed is 10 ~ 200sccm; Deposit film forms luminescent layer on described anode.
CN201310336806.3A 2013-08-05 2013-08-05 Alkali metal and titanium ion co-doped strontium selenide luminescent thin film, and preparation method and application thereof Pending CN104342157A (en)

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