CN103421490B - Cerium dopping alkaline earth lithium borate salt luminescent thin film, preparation method and application thereof - Google Patents
Cerium dopping alkaline earth lithium borate salt luminescent thin film, preparation method and application thereof Download PDFInfo
- Publication number
- CN103421490B CN103421490B CN201210151241.7A CN201210151241A CN103421490B CN 103421490 B CN103421490 B CN 103421490B CN 201210151241 A CN201210151241 A CN 201210151241A CN 103421490 B CN103421490 B CN 103421490B
- Authority
- CN
- China
- Prior art keywords
- thin film
- alkaline earth
- lithium borate
- borate salt
- substrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
A kind of cerium dopping alkaline earth lithium borate salt luminescent thin film, its chemical formula is MeLiBO3:xCe3+, wherein 0.005≤x≤0.05, MeLiBO3Being substrate, Ce elements is active element, and Me is Mg, Ca, Sr or Ba.In the electroluminescent spectrum (EL) of this cerium dopping alkaline earth lithium borate salt luminescent thin film, there is very strong glow peak in 535nm wavelength zone, it is possible to be applied in thin-film electroluminescent displays.The present invention also provides for preparation method and the application thereof of this cerium dopping alkaline earth lithium borate salt luminescent thin film.
Description
[technical field]
The present invention relates to a kind of cerium dopping alkaline earth lithium borate salt luminescent thin 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 big, Applicable temperature width, operation are simple, has caused and has paid close attention to widely, and quickly grown.At present, studying colored and to panchromatic TFELD, the thin film that exploitation multiband is luminous, is the developing direction of this problem.But, can be applicable to the cerium dopping alkaline earth lithium borate salt luminescent thin film of thin-film electroluminescent displays, have not yet to see report.
[summary of the invention]
Based on this, it is necessary to provide a kind of and can be applicable to the cerium dopping alkaline earth lithium borate salt luminescent thin film of membrane electro luminescent device, this cerium dopping alkaline earth lithium borate salt luminescent thin film electroluminescent device of its preparation method and preparation method thereof.
A kind of cerium dopping alkaline earth lithium borate salt luminescent thin film, its chemical formula is MeLiBO3:xCe3+, wherein MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba.
The preparation method of a kind of cerium dopping alkaline earth lithium borate salt luminescent thin film, comprises the following steps:
According to MeLiBO3:xCe3+The stoichiometric proportion of each element is by MeO, Li2O, B2O3And CeO2Powder body, after mixing, at 900 DEG C～1300 DEG C, sintering obtains target；
Substrate is loaded in the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to 1.0 × 10-3Pa～1.0 × 10-5Pa；
Regulating base target spacing is 45mm～95mm, substrate temperature is 250 DEG C～750 DEG C, and the flow of working gas is 10sccm～35sccm, and operating pressure is 0.2Pa～4Pa, pulsed laser energy is 50W～500W, and carrying out pulsed laser deposition, to obtain chemical formula be MeLiBO3:xCe3+Cerium dopping alkaline earth lithium borate salt luminescent thin film, wherein, MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba.
In a preferred embodiment, base target spacing is 60mm, and substrate temperature is 500 DEG C, and the flow of working gas is 25sccm, and operating pressure is 2Pa, and pulsed laser energy is 300W；
In a preferred embodiment, the thickness of cerium dopping alkaline earth lithium borate salt luminescent thin film is 80nm～500nm.
A kind of membrane electro luminescent device, this membrane electro luminescent device includes the substrate, anode layer, luminescent layer and the cathode layer that stack gradually, the material of described luminescent layer is cerium dopping alkaline earth lithium borate salt luminescent thin film, and the chemical formula of this cerium dopping alkaline earth lithium borate salt luminescent thin film is MeLiBO3:xCe3+, wherein MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba.
The preparation method of a kind of membrane electro luminescent device, comprises the following steps:
The substrate with anode is provided；
Forming luminescent layer on described anode, the material of described luminescent layer is cerium dopping alkaline earth lithium borate salt luminescent thin film, and the chemical formula of this cerium dopping alkaline earth lithium borate salt luminescent thin film is MeLiBO3:xCe3+, wherein, MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba；
Form negative electrode on the light-emitting layer.
In a preferred embodiment, the preparation of described luminescent layer comprises the following steps:
According to MeLiBO3:xCe3+The stoichiometric proportion of each element is by MeO, Li2O, B2O3And CeO2Powder body, after mixing, at 900 DEG C～1300 DEG C, sintering obtains target；
Substrate is loaded in the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to 1.0 × 10-3Pa～1.0 × 10-5Pa；
Regulating base target spacing is 45mm～95mm, substrate temperature is 250 DEG C～750 DEG C, and the flow of working gas is 10sccm～35sccm, and operating pressure is 0.2Pa～4Pa, pulsed laser energy is 50W～500W, and carrying out pulsed laser deposition, to obtain chemical formula be MeLiBO3:xCe3+Cerium dopping alkaline earth lithium borate salt luminescent thin film, wherein MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba.
Above-mentioned cerium dopping alkaline earth lithium borate salt luminescent thin film (MeLiBO3:xCe3+) electroluminescent spectrum (EL) in, have very strong glow peak in 535nm wavelength zone, it is possible to 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 electroluminescent spectrogram of the cerium dopping alkaline earth lithium borate salt luminescent thin film of embodiment 1 preparation；
Fig. 3 is the XRD figure of the cerium dopping alkaline earth lithium borate salt luminescent thin film of embodiment 1 preparation.
Fig. 4 is voltage and electric current and the brightness relationship figure of the membrane electro luminescent device of embodiment 1 preparation.
[detailed description of the invention]
Below in conjunction with the drawings and specific embodiments, cerium dopping alkaline earth lithium borate salt luminescent thin film, its preparation method and membrane electro luminescent device and preparation method thereof are further elucidated with.
The cerium dopping alkaline earth lithium borate salt luminescent thin film of one embodiment, its chemical formula is MeLiBO3:xCe3+, wherein MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba.
Preferably, the thickness of cerium dopping alkaline earth lithium borate salt luminescent thin film is 80nm～500nm, x is 0.02.
It is furthermore preferred that the thickness of cerium dopping alkaline earth lithium borate salt luminescent thin film is 250nm.
MeLiBO in this cerium dopping alkaline earth lithium borate salt luminescent thin film3Being substrate, Ce elements is active element.In the electroluminescent spectrum (EL) of this cerium dopping alkaline earth lithium borate salt luminescent thin film, there is very strong glow peak in 535nm wavelength zone, it is possible to be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned cerium dopping alkaline earth lithium borate salt luminescent thin film, comprises the following steps:
Step S11, according to MeLiBO3:xCe3+The stoichiometric proportion of each element is by MeO, Li2O, B2O3And CeO2Powder body, after mixing, at 900 DEG C～1300 DEG C, sintering obtains target；Substrate is loaded in the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to 1.0 × 10-2Pa～1.0 × 10-3Pa。
In the present embodiment, substrate is indium tin oxide glass (ITO), it is appreciated that in other embodiments, it is also possible to for fluorine doped tin oxide glass (FTO), the zinc oxide (AZO) mixing aluminum or indium-doped zinc oxide (IZO)；Substrate successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, sends into reative cell after nitrogen is air-dry；
Preferably, at 1250 DEG C, sintering obtains target；The vacuum of reative cell is 5.0 × 10-4Pa。
Step S13, adjustment base target spacing are 45mm～95mm, substrate temperature is 250 DEG C～750 DEG C, and the flow of working gas is 10sccm～35sccm, and operating pressure is 0.2Pa～4Pa, pulsed laser energy is 50W～500W, and carrying out pulsed laser deposition, to obtain chemical formula be MeLiBO3:xCe3+Cerium dopping alkaline earth lithium borate salt luminescent thin film, wherein, MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba；
In a preferred embodiment, base target spacing is 60mm, and substrate temperature is 500 DEG C, and the flow of working gas is 25sccm, and operating pressure is 2Pa, and pulsed laser energy is 300W；
In a preferred embodiment, the thickness of cerium dopping alkaline earth lithium borate salt luminescent thin film is 80nm～500nm；
Step S14, then passing to oxygen, carrying out chemical vapour deposition (CVD), to obtain its chemical formula of cerium dopping alkaline earth lithium borate salt luminescent thin film be MeLiBO3:xCe3+, wherein MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba.
Referring to Fig. 1, the membrane electro luminescent device 100 of an embodiment, this membrane electro luminescent device 100 includes the substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 that stack gradually.
Substrate 1 is glass substrate.Anode 2 is the tin indium oxide (ITO) being formed in glass substrate.The material of luminescent layer 3 is cerium dopping alkaline earth lithium borate salt luminescent thin film, and the chemical formula of this cerium dopping alkaline earth lithium borate salt luminescent thin film is MeLiBO3:xCe3+, wherein MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba.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 there is the substrate 1 of anode 2.
In present embodiment, substrate 1 is glass substrate, and anode 2 is the tin indium oxide (ITO) being formed in glass substrate.It is appreciated that in other embodiments, it is also possible to for fluorine doped tin oxide glass (FTO), the zinc oxide (AZO) mixing aluminum or indium-doped zinc oxide (IZO)；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 formed luminescent layer 3, the material of luminescent layer 3 is cerium dopping alkaline earth lithium borate salt luminescent thin film, and the chemical formula of this cerium dopping alkaline earth lithium borate salt luminescent thin film is MeLiBO3:xCe3+, wherein MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba.
In present embodiment, luminescent layer 3 is prepared by following steps:
First, according to MeLiBO3:xCe3+The stoichiometric proportion of each element is by MeO, Li2O, B2O3And CeO2Powder body, after mixing, at 900 DEG C～1300 DEG C, sintering obtains target；
Substrate is loaded in the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to 1.0 × 10-3Pa～1.0 × 10-5Pa,
Moreover, regulate base target spacing be 45mm～95mm, substrate temperature is 250 DEG C～750 DEG C, and the flow of working gas is 10sccm～35sccm, and operating pressure is 0.2Pa～4Pa, pulsed laser energy is 50W～500W, and carrying out pulsed laser deposition, to obtain chemical formula be MeLiBO3:xCe3+Cerium dopping alkaline earth lithium borate salt luminescent thin film, wherein MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba.
In a preferred embodiment, base target spacing is 60mm, and substrate temperature is 500 DEG C, and the flow of working gas is 25sccm, and operating pressure is 2Pa, and pulsed laser energy is 300W；
Step S23, on luminescent layer 3 formed negative electrode 4.
In present embodiment, the material of negative electrode 4 is silver (Ag), evaporation formed.
It is specific embodiment below.
Embodiment 1
By 1molMgO, 0.5molLi2O, 0.5molB2O3And 0.02molCeO2Powder body is after Homogeneous phase mixing, sinter at 1250 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm is the shape of cake, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 60mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 5.0 × 10-4Pa；Adopting argon as working air current, working gas flow is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, pulsed laser energy 300W, starts the deposition of thin film.The thickness deposition of thin film is to 250nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is MgLiBO3:0.02Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
The chemical general formula of the cerium dopping alkaline earth lithium borate salt luminescent thin film obtained in the present embodiment is MgLiBO3:0.02Ce3+, wherein MgLiBO3Being substrate, Ce elements is active element.
Refer to Fig. 2, Fig. 2 and show the electroluminescence spectrum (EL) of the cerium dopping alkaline earth lithium borate salt luminescent thin film obtained.As seen from Figure 2, in electroluminescence spectrum, there is very strong glow peak can be applied in thin-film electroluminescent displays in 535nm ripple caliper zones.
Refer to the XRD curve of the cerium dopping alkaline earth lithium borate salt luminescent thin film that Fig. 3, Fig. 3 are embodiment 1 preparation, test comparison standard PDF card.As can be seen from Figure 3 diffraction maximum is all the peak crystallization that lithium borate salt is relevant, it does not have the diffraction maximum of doped chemical and other impurity occur.
Refer to Fig. 4, Fig. 4 is voltage and electric current and the brightness relationship figure of the membrane electro luminescent device of embodiment 1 preparation, and curve 1 is voltage and electric current density relation curve in figure 4, it can be seen that device starts luminescence from 5.5V, curve 2 is voltage and brightness relationship curve, and high-high brightness is 79cd/m2, it was shown that device has the good characteristics of luminescence.
Embodiment 2
By 1molMgO, 0.5molLi2O, 0.5molB2O3And 0.05molCeO2Powder body is after Homogeneous phase mixing, sinter at 900 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 60mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 1.0 × 10-3Pa；Adopting argon as working air current, working gas flow is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C, pulsed laser energy 500W, starts the deposition of thin film.The thickness deposition of thin film is to 80nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is MgLiBO3:0.05Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 3
By 1molMgO, 0.5molLi2O, 0.5molB2O3And 0.005molCeO2Powder body is after Homogeneous phase mixing, sinter at 1300 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 95mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 1.0 × 10-5Pa；Adopting argon as working air current, working gas flow is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, pulsed laser energy 50W, starts the deposition of thin film.The thickness deposition of thin film is to 500nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is MgLiBO3: 0.005Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 4
By 1molCaO, 0.5molLi2O, 0.5molB2O3And 0.02molCeO2Powder body is after Homogeneous phase mixing, sinter at 1250 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 60mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 5.0 × 10-4Pa；Adopting argon as working air current, working gas flow is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, pulsed laser energy 300W, starts the deposition of thin film.The thickness deposition of thin film is to 400nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is CaLiBO3:0.02Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 5
By 1molCaO, 0.5molLi2O, 0.5molB2O3And 0.05molCeO2Powder body is after Homogeneous phase mixing, sinter at 900 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 45mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 1.0 × 10-3Pa；Adopting argon as working air current, working gas flow is 10sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 250 DEG C, pulsed laser energy 500W, starts the deposition of thin film.The thickness deposition of thin film is to 300nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is CaLiBO3:0.05Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 6
By 1molCaO, 0.5molLi2O, 0.5molB2O3And 0.005molCeO2Powder body is after Homogeneous phase mixing, sinter at 1300 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 95mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 1.0 × 10-5Pa；Adopting argon as working air current, working gas flow is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, pulsed laser energy 50W, starts the deposition of thin film.The thickness deposition of thin film is to 200nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is CaLiBO3:0.005Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 7
By 1molSrO, 0.5molLi2O, 0.5molB2O3And 0.02molCeO2Powder body is after Homogeneous phase mixing, sinter at 1250 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 60mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 5.0 × 10-4Pa；Adopting argon as working air current, working gas flow is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, pulsed laser energy 300W, starts the deposition of thin film.The thickness deposition of thin film is to 250nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is SrLiBO3:0.02Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 8
By 1molSrO, 0.5molLi2O, 0.5molB2O3And 0.05molCeO2Powder body is after Homogeneous phase mixing, sinter at 900 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 45mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 1.0 × 10-3Pa；Adopting argon as working air current, working gas flow is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C, pulsed laser energy 500W, starts the deposition of thin film.The thickness deposition of thin film is to 100nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is SrLiBO3:0.05Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 9
By 1molSrO, 0.5molLi2O, 0.5molB2O3And 0.005molCeO2Powder body is after Homogeneous phase mixing, sinter at 1300 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 95mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 1.0 × 10-5Pa；Adopting argon as working air current, working gas flow is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, pulsed laser energy 50W, starts the deposition of thin film.The thickness deposition of thin film is to 150nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is SrLiBO3:0.005Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 10
By 1molBaO, 0.5molLi2O, 0.5molB2O3And 0.02molCeO2Powder body is after Homogeneous phase mixing, sinter at 1250 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 60mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 5.0 × 10-4Pa；Adopting argon as working air current, working gas flow is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, pulsed laser energy 300W, starts the deposition of thin film.The thickness deposition of thin film is to 130nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is BaLiBO3:0.02Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 11
By 1molBaO, 0.5molLi2O, 0.5molB2O3And 0.05molCeO2Powder body is after Homogeneous phase mixing, sinter at 900 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 45mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 1.0 × 10-3Pa；Adopting argon as working air current, working gas flow is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C, pulsed laser energy 500W, starts the deposition of thin film.The thickness deposition of thin film is to 220nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is BaLiBO3:0.05Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 12
By 1molBaO, 0.5molLi2O, 0.5molB2O3And 0.005molCeO2Powder body is after Homogeneous phase mixing, sinter at 1300 DEG C and be of a size of diameter 50, thickness is the ceramic target of 2mm, and target is loaded in vacuum cavity, it is ito glass by substrate, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, and carry out oxygen plasma treatment with to it, put into vacuum cavity.The distance of target and substrate is set as 95mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 1.0 × 10-5Pa；Adopting argon as working air current, working gas flow is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, pulsed laser energy 50W, starts the deposition of thin film.The thickness deposition of thin film is to 420nm, and the chemical general formula taking out the cerium dopping alkaline earth lithium borate salt luminescent thin film that sample obtains is BaLiBO3:0.005Ce3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment described above only have expressed the several embodiments 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, it is also possible to making some deformation and improvement, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (5)
1. the preparation method of a cerium dopping alkaline earth lithium borate salt luminescent thin film, it is characterised in that comprise the following steps:
According to MeLiBO3: xCe3+The stoichiometric proportion of each element is by MeO, Li2O, B2O3And CeO2Powder body, after mixing, at 900 DEG C～1300 DEG C, sintering obtains target；
Substrate is loaded in the reative cell of pulsed laser deposition equipment, and the vacuum of reative cell is set to 1.0 × 10-3Pa～1.0 × 10-5Pa；
Regulating base target spacing is 45mm～95mm, substrate temperature is 250 DEG C～750 DEG C, and the flow of working gas is 10sccm～35sccm, and operating pressure is 0.2Pa～4Pa, pulsed laser energy is 50W～500W, and carrying out pulsed laser deposition, to obtain chemical formula be MeLiBO3: xCe3+Cerium dopping alkaline earth lithium borate salt luminescent thin film, wherein, MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba.
2. the preparation method of cerium dopping alkaline earth lithium borate salt luminescent thin film according to claim 1, it is characterised in that described base target spacing is 60mm, substrate temperature is 500 DEG C, the flow of working gas is 25sccm, and operating pressure is 2Pa, and pulsed laser energy is 300W.
3. the preparation method of cerium dopping alkaline earth lithium borate salt luminescent thin film according to claim 1, it is characterised in that the thickness of described cerium dopping alkaline earth lithium borate salt luminescent thin film is 80nm～500nm.
4. the preparation method of a membrane electro luminescent device, it is characterised in that comprise the following steps:
The substrate with anode is provided；
Forming luminescent layer on described anode, the thin film of described luminescent layer is cerium dopping alkaline earth lithium borate salt luminescent thin film, and the chemical formula of this cerium dopping alkaline earth lithium borate salt luminescent thin film is MeLiBO3: xCe3+, wherein, MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba；The preparation of described luminescent layer comprises the following steps:
According to MeLiBO3: xCe3+The stoichiometric proportion of each element is by MeO, Li2O, B2O3And CeO2Powder body, after mixing, at 900 DEG C～1300 DEG C, sintering obtains target；
Described substrate is loaded the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to 1.0 × 10-3Pa～1.0 × 10-5Pa；
Regulating base target spacing is 45mm～95mm, substrate temperature is 250 DEG C～750 DEG C, and the flow of working gas is 10sccm～35sccm, and operating pressure is 0.2Pa～4Pa, pulsed laser energy is 50W～500W, and carrying out pulsed laser deposition, to obtain chemical formula be MeLiBO3: xCe3+Cerium dopping alkaline earth lithium borate salt luminescent thin film, wherein MeLiBO3Being substrate, Ce elements is active element, 0.005≤x≤0.05, and Me is Mg, Ca, Sr or Ba；
Form negative electrode on the light-emitting layer.
5. the preparation method of membrane electro luminescent device according to claim 4, it is characterised in that described base target spacing is 60mm, and substrate temperature is 500 DEG C, and the flow of working gas is 25sccm, and operating pressure is 2Pa, and pulsed laser energy is 300W.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210151241.7A CN103421490B (en) | 2012-05-16 | 2012-05-16 | Cerium dopping alkaline earth lithium borate salt luminescent thin film, preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210151241.7A CN103421490B (en) | 2012-05-16 | 2012-05-16 | Cerium dopping alkaline earth lithium borate salt luminescent thin film, preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103421490A CN103421490A (en) | 2013-12-04 |
| CN103421490B true CN103421490B (en) | 2016-06-29 |
Family
ID=49646891
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210151241.7A Active CN103421490B (en) | 2012-05-16 | 2012-05-16 | Cerium dopping alkaline earth lithium borate salt luminescent thin film, preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103421490B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101793969A (en) * | 2010-04-09 | 2010-08-04 | 中国科学院长春应用化学研究所 | Application of LiCaBO3: Ce3+ for preparing thermoluminescent dosemeter |
-
2012
- 2012-05-16 CN CN201210151241.7A patent/CN103421490B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101793969A (en) * | 2010-04-09 | 2010-08-04 | 中国科学院长春应用化学研究所 | Application of LiCaBO3: Ce3+ for preparing thermoluminescent dosemeter |
Non-Patent Citations (7)
| Title |
|---|
| Ce3+在LiBaBO3中的发光特性及晶体学格位;李盼来 等;《物理化学》;20090815;第58卷(第8期);5831-5835 * |
| Ce3+在碱金属-碱土金属硼酸盐体系中的光谱特征;王志军等;《光谱学与光谱分析》;20100315;第30卷(第3期);735-737 * |
| Ce3+激活的LiSrBO3材料发光特性及晶体学格位研究;李盼来等;《高等学校化学学报》;20090810;第30卷(第8期);1487-1491 * |
| Luminescent characteristics of LiSrBO3:M (M = Eu3+, Sm3+, Tb3+, Ce3+, Dy3+)phosphor for white light-emitting diode;Panlai Li 等;《Materials Research Bulletin》;20090723;第44卷;2068-2071 * |
| PanlaiLi 等.LuminescentcharacteristicsofLiCaBo3:M (M ¼Eu3+, Sm3+, Tb3+, Ce3+, Dy3+) phosphor for white LED.《Journal ofLuminescence》.2009,第130卷222-225. * |
| ThermoluminescencestudiesofLiSrBO3:RE3+(RE=Dy,Tb,Tm and Ce);L.H. Jiang等;《Applied RadiationandIsotopes》;20091005;第68卷;196-200 * |
| 白光LED用LiCaBO3:Ce3+材料发光特性研究;李盼来 等;《科学通报》;20090408;第54卷(第7期);866-870 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103421490A (en) | 2013-12-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103805192A (en) | Samarium-doped rare earth borate luminous film as well as preparation method and application thereof | |
| CN102863961A (en) | Cerium-doped yttrium-aluminum borate luminescent material, preparation method and application thereof | |
| CN103421490B (en) | Cerium dopping alkaline earth lithium borate salt luminescent thin film, preparation method and application thereof | |
| CN103805183A (en) | Europium-erbium double-doped zirconium dioxide light-emitting film and preparation method and application thereof | |
| CN103805172A (en) | Cerium-terbium co-doped calcium sulfate luminous film and preparation method and application thereof | |
| CN104650884A (en) | Luminescent film, preparation method and application thereof | |
| CN103805186A (en) | Copper-iridium co-doped vanadate light-emitting film, and preparation method and application thereof | |
| CN103668064A (en) | Aluminum and gallium co-doped zinc oxide conductive thin film, as well as preparation method and application thereof | |
| CN106147764A (en) | A kind of manganese-chromium-codoped zirconium arsenate light-emitting film, preparation method and applications | |
| CN103571475A (en) | Titanium manganese-codoped group-III molybdate luminescent material, preparation method and application thereof | |
| CN103421499B (en) | Additive Mn arsenate light-emitting film, preparation method and application thereof | |
| CN104119894A (en) | Titanium-doped alkaline earth borophosphate luminescent thin film and preparation method and application thereof | |
| CN103571476A (en) | Cerium-doped Group-III molybdate light-emitting film, preparation method and application thereof | |
| CN104342139A (en) | Titanium and manganese co-doped vanadium silicate luminescent material, preparation method and application of luminescent material | |
| CN104140812A (en) | III-group scandium silicate luminescent material co-doped with titanium and manganese, preparing method thereof and applications of the material | |
| CN104650918A (en) | Europium- bismuth- co-doped IIIA-group yttrium fluoride luminescent materials, and preparing method and applications thereof | |
| CN103805189A (en) | Manganese-chromium-codoped alkaline earth titanium phosphate light-emitting thin film as well as preparation method and application thereof | |
| CN103289688B (en) | titanium doped aluminate luminescent film, preparation method and application thereof | |
| CN103805187A (en) | Samarium-doped alkaline earth vanadate luminous film and preparation method and application thereof | |
| CN104119906A (en) | Antimony terbium co-doped silicon nitride luminescent material and preparation method and application thereof | |
| CN103805193A (en) | Cerium-doped rare earth borate light-emitting film and preparation method and application thereof | |
| CN103571477A (en) | Europium bismuth co-doped Group-III molybdate light-emitting material, preparation method and application thereof | |
| CN103805188A (en) | Cerium and terbium codoped borophosphate light-emitting film as well as preparation method and application of cerium and terbium codoped borophosphate light-emitting film | |
| CN103805185A (en) | Praseodymium-doped molybdate light emitting film and preparation method and application thereof | |
| CN104277832A (en) | Europium and terbium-co-doped vanadite luminescent thin film and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |