CN104673309A - Scandium titanate luminescent material and preparation method and application thereof - Google Patents
Scandium titanate luminescent material and preparation method and application thereof Download PDFInfo
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- CN104673309A CN104673309A CN201310616785.0A CN201310616785A CN104673309A CN 104673309 A CN104673309 A CN 104673309A CN 201310616785 A CN201310616785 A CN 201310616785A CN 104673309 A CN104673309 A CN 104673309A
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- titanate luminescent
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Abstract
The invention provides a scandium titanate luminescent material and a preparation method and application thereof. The scandium titanate luminescent material provided by the invention has the structural formula of R2Sc2Ti3O12:xMn<4+>, wherein R is Al, Ga, In or Tl, and x is 0.01-0.05. The scandium titanate luminescent material has good structural stability, has very strong luminescence peaks near a 650nm position, and has attractive application prospects in the fields of luminescence and display technologies, laser and photoelectronics technologies, detecting technologies and the like. The invention further provides a thin-film electroluminescent device and a preparation method thereof.
Description
Technical field
The present invention relates to phosphor field, particularly relate to a kind of scandium titanate luminescent film and its preparation method and application.
Background technology
Compared with the display screen made with traditional luminescent powder, light-emitting film contrast gradient, resolving power, thermal conduction, homogeneity, with the tack, outgas speed etc. of substrate in all demonstrate stronger superiority.Therefore, as functional materials, light-emitting film has broad application prospects in the flat display field such as such as cathode tube (CRTs), electroluminance display (ELDs) and Field Emission Display (FEDs).
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 material of exploitation multiband luminescence is the developing direction of this problem.But scandium titanate luminescent film has not yet to see report.
Summary of the invention
In order to solve the problem, the invention provides a kind of scandium titanate luminescent material, scandium titanate luminescent material provided by the invention is preferably scandium titanate luminescent film, present invention also offers the preparation method and application of this scandium titanate luminescent material.
First aspect, the invention provides a kind of scandium titanate luminescent material, and structural formula is R
2sc
2ti
3o
12: xMn
4+, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05.
In described scandium titanate, with R
2sc
2ti
3o
12for matrix, Mn
4+for active element, R
2sc
2ti
3o
12matrix has higher calorifics and mechanical stability, and good optical transparence and lower phonon energy, for light emitting ionic provides excellent crystal field, thus less radiationless transition is produced in the process of photovoltaic energy conversion, therefore, it is as photoelectric conversion material, little power consumption, and transform light energy rate is high.For dopant ion, transition metal ion Mn
4+have abundant energy level and the narrow spectral line of emission, combine can form different glow peaks from matrix, in this system, the 650nm luminescence of material is the SP from substrate material
3hybridized orbital electronics is to Mn
4+3d
5the transmission ofenergy of electronics, the red light-emitting peak given off.
Preferably, the value of described x is 0.03.
Preferably, described scandium titanate luminescent material is light-emitting film.The thickness of light-emitting film can be prepared according to actual needs.Preferably, the thickness of described light-emitting film is 50 ~ 350nm.
More preferably, the thickness of described light-emitting film is 160nm.
The present invention has prepared the scandium titanate luminescent material R of additive Mn
2sc
2ti
3o
12: xMn
4+, with R
2sc
2ti
3o
12for matrix, Mn
4+for active element, serve as main luminescence center in the material.The scandium titanate luminescent material R of additive Mn provided by the invention
2sc
2ti
3o
12: xMn
4+very strong green luminescence peak is had near 520nm position.
Second aspect, the invention provides a kind of preparation method of scandium titanate luminescent material, comprises the following steps:
According to R
2sc
2ti
3o
12: xMn
4+the stoichiometric ratio of each element provides or prepares ceramic target, and wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05;
Substrate and described ceramic target are placed in the vacuum film coating chamber of magnetron sputtering equipment, arranging vacuum tightness is 1.0 × 10
-3~ 1.0 × 10
-5pa, underlayer temperature is 250 ~ 750 DEG C, distance between described substrate and ceramic target is 45 ~ 95mm, pass into 10 ~ 35sccm argon gas, under the pressure of 0.2 ~ 4Pa, adopt the method for magnetron sputtering to deposit over the substrate and obtain scandium titanate luminescent material, wherein, the power of magnetron sputtering is 30 ~ 200W;
The structural formula of described scandium titanate luminescent material is R
2sc
2ti
3o
12: xMn
4+, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05.
The present invention adopts the method for magnetron sputtering to prepare scandium titanate luminescent material, first provides or prepares ceramic target, then carries out magnetron sputtering deposition and obtain luminescent material.
Preferably, the step provided described in or prepare ceramic target comprises:
R is taken respectively by the mol ratio of 1: 1: 3: x
2o
3, Sc
2o
3, TiO
2, MnO
2powder, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05;
Insert in roasting assembly after the above-mentioned powder taken is mixed, calcine 0.5 ~ 3 hour at 900 ~ 1300 DEG C, obtain Bulk ceramic target.
Further preferably, insert in roasting assembly in the process of carrying out calcining after being mixed by described powder, described calcining temperature is 1250 DEG C, and calcination time is 1.5.
Preferably, the size of the Bulk ceramic target of described acquisition is Φ 50 × 2mm.
Preferably, the value of described x is 0.03.
Preferably, the vacuum tightness of the vacuum film coating chamber of described magnetron sputtering equipment is 5.0 × 10
-4pa.
Preferably, described substrate is glass.
Preferably, described substrate temperature is 500 DEG C.
Preferably, the distance between described substrate and ceramic target is 60mm.
Preferably, describedly obtain in the process of described scandium titanate luminescent material at deposited on substrates, the pressure of vacuum plating indoor is 2Pa.
Preferably, the power of described magnetron sputtering is 120W.
Preferably, the time of described deposition is 10 ~ 30min.
Preferably, the flow of described argon gas is 25sccm.
The scandium titanate luminescent material of above-mentioned preparation is light-emitting film.Light-emitting film can prepare different thickness according to actual needs.Preferably, the thickness of described light-emitting film is 50 ~ 350nm.
More preferably, the thickness of described light-emitting film is 160nm.
Preferably, describedly obtain in the process of scandium titanate luminescent material at deposited on substrates, comprise the anneal to gained scandium titanate luminescent material, the mode of described anneal is: after deposited on substrates scandium titanate luminescent material, the pressure of adjustment vacuum plating indoor is 0.001 ~ 0.1Pa, under an argon atmosphere, anneal 1 ~ 3 hour at 500 ~ 800 DEG C.
Preferably, annealing temperature is 600 DEG C.Preferably, annealing time is 2 hours.
The third aspect, the invention provides a kind of membrane electro luminescent device, and this membrane electro luminescent device comprises substrate, anode, luminescent layer and negative electrode, and the material of described luminescent layer is scandium titanate luminescent material, and the structural formula of described scandium titanate luminescent material is R
2sc
2ti
3o
12: xMn
4+, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05.
Preferably, the value of described x is 0.03.
Preferably, described substrate is glass.Preferably, described anode is ito thin film.Preferably, the material of described negative electrode is silver.
Described scandium titanate luminescent material is light-emitting film.The thickness of light-emitting film can be prepared according to actual needs.Preferably, the thickness of described light-emitting film is 50 ~ 350nm.
More preferably, the thickness of described light-emitting film is 160nm.
Fourth aspect, the invention provides a kind of preparation method of membrane electro luminescent device, comprises the following steps:
According to R
2sc
2ti
3o
12: xMn
4+the stoichiometric ratio of each element provides or prepares ceramic target, and wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05;
Substrate and described ceramic target are placed in the vacuum film coating chamber of magnetron sputtering equipment, arranging vacuum tightness is 1.0 × 10
-3~ 1.0 × 10
-5pa, underlayer temperature is 250 ~ 750 DEG C, distance between described substrate and ceramic target is 45 ~ 95mm, pass into 10 ~ 35sccm argon gas, under the pressure of 0.2 ~ 4Pa, adopt the method for magnetron sputtering to deposit over the substrate and obtain scandium titanate luminescent material, wherein, the power of magnetron sputtering is 30 ~ 200W;
The structural formula of described scandium titanate luminescent material is R
2sc
2ti
3o
12: xMn
4+, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05;
Evaporation negative electrode on described scandium titanate luminescent material, obtains membrane electro luminescent device again.
Preferably, the step provided described in or prepare ceramic target comprises:
R is taken respectively by the mol ratio of 1: 1: 3: x
2o
3, Sc
2o
3, TiO
2, MnO
2powder, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05;
Insert in roasting assembly after the above-mentioned powder taken is mixed, calcine 0.5 ~ 3 hour at 900 ~ 1300 DEG C, obtain Bulk ceramic target.
Further preferably, insert in roasting assembly in the process of carrying out calcining after being mixed by described powder, described calcining temperature is 1250 DEG C, and calcination time is 1.5h.
Preferably, the size of the Bulk ceramic target of described acquisition is Φ 50 × 2mm.
Preferably, the value of described x is 0.03.
Preferably, the vacuum tightness of the vacuum film coating chamber of described magnetron sputtering equipment is 5.0 × 10
-4pa.
Preferably, described substrate is glass.
Preferably, described substrate temperature is 500 DEG C.
Preferably, the distance between described substrate and ceramic target is 60mm.
Preferably, describedly obtain in the process of described scandium titanate luminescent material at deposited on substrates, the pressure of vacuum plating indoor is 2Pa.
Preferably, the power of described magnetron sputtering is 120W.
Preferably, the time of described deposition is 10 ~ 30min.
Preferably, the flow of described argon gas is 25sccm.
Described scandium titanate luminescent material is light-emitting film.Light-emitting film can prepare different thickness according to actual needs.Preferably, the thickness of described light-emitting film is 50 ~ 350nm.
More preferably, the thickness of described light-emitting film is 160nm.
Preferably, describedly obtain in the process of scandium titanate luminescent material at deposited on substrates, comprise the anneal to gained scandium titanate luminescent material, the mode of described anneal is: after deposited on substrates scandium titanate luminescent material, the pressure of adjustment vacuum plating indoor is 0.001 ~ 0.1Pa, under an argon atmosphere, anneal 1 ~ 3 hour at 500 ~ 800 DEG C.
Preferably, annealing temperature is 600 DEG C.Preferably, annealing time is 2 hours.
Preferably, the material of described negative electrode is silver.
The scandium titanate luminescent material R of additive Mn provided by the invention
2sc
2ti
3o
12: xMn
4+, with R
2sc
2ti
3o
12for matrix, Mn
4+for active element, serve as main luminescence center in the material.The scandium titanate luminescent material R of additive Mn provided by the invention
2sc
2ti
3o
12: xMn
4+very strong green luminescence peak is had near 520nm position.This luminescent material has tempting application prospect luminous with technique of display, laser and the field such as photoelectron technology and Detection Techniques.In addition, the preparation method of scandium titanate luminescent film provided by the invention adopts the method for magnetron sputtering, the product thickness obtained is even, quality of forming film is high, defect is few, luminous efficiency is high, and condition is easy to control, have good operability, accurately can control thickness and the shape size of film.
Accompanying drawing explanation
Fig. 1 is the electroluminescent spectrum figure of luminescent material prepared by the embodiment of the present invention 1;
Fig. 2 is the XRD figure of luminescent material prepared by the embodiment of the present invention 1;
The structural representation of the membrane electro luminescent device that Fig. 3 provides for the embodiment of the present invention 13;
Fig. 4 is the voltage of membrane electro luminescent device prepared of embodiment 13 and electric current and brightness relationship figure.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of scandium titanate luminescent material, structural formula is Al
2sc
2ti
3o
12: 0.03Mn
4+, obtain by the following method:
Take 1mmol respectively, the Al of 1mmol, 3mmol, 0.03mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 1250 DEG C, calcine 1.5h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranged between described substrate and described ceramic target is 60mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 5.0 × 10
-4pa, underlayer temperature is 500 DEG C, then passes into argon gas, airshed is 25sccm, and under the operating pressure of 2Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 120W, depositing time is 30min, after deposition terminates, under 0.01Pa pressure, in argon gas atmosphere, anneal 2 hours at 600 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is Al
2sc
2ti
3o
12: 0.03Mn
4+, be light-emitting film, light-emitting film thickness is 160nm.
Fig. 1 is the electroluminescent spectrum figure of luminescent material prepared by the embodiment of the present invention 1.As we can see from the figure, structural formula is Al
2sc
2ti
3o
12: 0.03Mn
4+sample near the position of 650nm, have obvious glow peak, this is the SP from substrate material
3hybridized orbital electronics is to Mn
4+3d
5the transmission ofenergy of electronics, the red light-emitting peak given off.
Fig. 2 is the XRD curve of luminescent material prepared by embodiment 1, test comparison standard P DF card.As can be seen from Figure 1 in figure X-ray diffraction peak corresponding be the characteristic peak of scandium titanate, do not occur doped element and the relevant peak of impurity, illustrate that additive Mn ion enters the lattice of scandium titanate, sample has good crystallographic property.
Embodiment 2
A kind of scandium titanate luminescent material, structural formula is Al
2sc
2ti
3o
12: 0.01Mn
4+, obtain by the following method:
Take 1mmol respectively, the Al of 1mmol, 3mmol, 0.01mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 900 DEG C, calcine 0.5h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 45mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-3pa, underlayer temperature is 250 DEG C, then passes into argon gas, airshed is 10sccm, and under the operating pressure of 0.2Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 30W, depositing time is 10min, after deposition terminates, under 0.1Pa pressure, in argon gas atmosphere, anneal 1 hour at 500 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is Al
2sc
2ti
3o
12: 0.01Mn
4+, be light-emitting film, light-emitting film thickness is 50nm.
Embodiment 3
A kind of scandium titanate luminescent material, structural formula is Al
2sc
2ti
3o
12: 0.05Mn
4+, obtain by the following method:
Take 1mmol respectively, the Al of 1mmol, 3mmol, 0.05mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 1300 DEG C, calcine 3h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 95mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-5pa, underlayer temperature is 750 DEG C, then passes into argon gas, airshed is 35sccm, under the operating pressure of 4Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, and the power of magnetron sputtering is 200W, depositing time is 15min, after deposition terminates, at the ar pressure of 0.001Pa, and anneal 3 hours at the temperature of 800 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is Al
2sc
2ti
3o
12: 0.05Mn
4+, be light-emitting film, light-emitting film thickness is 320nm.
Embodiment 4
A kind of scandium titanate luminescent material, structural formula is Ga
2sc
2ti
3o
12: 0.03Mn
4+, obtain by the following method:
Take 1mmol respectively, the Ga of 1mmol, 3mmol, 0.03mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 1250 DEG C, calcine 2h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 60mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 5.0 × 10
-4pa, underlayer temperature is 500 DEG C, then passes into argon gas, airshed is 25sccm, and under the operating pressure of 2Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 30W, depositing time is 10min, after deposition terminates, under 0.01Pa pressure, in argon gas atmosphere, anneal 2 hours at 600 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is Ga
2sc
2ti
3o
12: 0.03Mn
4+, be light-emitting film, light-emitting film thickness is 150nm.
Embodiment 5
A kind of scandium titanate luminescent material, structural formula is Ga
2sc
2ti
3o
12: 0.01Mn
4+, obtain by the following method:
Take 1mmol respectively, the Ga of 1mmol, 3mmol, 0.01mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 900 DEG C, calcine 0.5h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 45mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-3pa, underlayer temperature is 250 DEG C, then passes into argon gas, airshed is 10sccm, and under the operating pressure of 0.2Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 80W, depositing time is 30min, after deposition terminates, under 0.1Pa pressure, in argon gas atmosphere, anneal 1 hour at 500 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is Ga
2sc
2ti
3o
12: 0.01Mn
4+, be light-emitting film, light-emitting film thickness is 60nm.
Embodiment 6
A kind of scandium titanate luminescent material, structural formula is Ga
2sc
2ti
3o
12: 0.05Mn
4+, obtain by the following method:
Take 1mmol respectively, the Ga of 1mmol, 3mmol, 0.05mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 1300 DEG C, calcine 2.5h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 95mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-5pa, underlayer temperature is 750 DEG C, then passes into argon gas, airshed is 35sccm, and under the operating pressure of 4Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 100W, depositing time is 30min, after deposition terminates, under 0.06Pa pressure, in argon gas atmosphere, anneal 3 hours at 800 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is Ga
2sc
2ti
3o
12: 0.05Mn
4+, be light-emitting film, light-emitting film thickness is 350nm.
Embodiment 7
A kind of scandium titanate luminescent material, structural formula is In
2sc
2ti
3o
12: 0.03Mn
4+, obtain by the following method:
Take 1mmol respectively, the In of 1mmol, 3mmol, 0.03mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 1250 DEG C, calcine 2h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 60mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 5.0 × 10
-4pa, underlayer temperature is 500 DEG C, then passes into argon gas, airshed is 25sccm, and under the operating pressure of 2Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 180W, depositing time is 10min, after deposition terminates, under 0.01Pa pressure, in argon gas atmosphere, anneal 2 hours at the temperature of 600 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is In
2sc
2ti
3o
12: 0.03Mn
4+, be light-emitting film, light-emitting film thickness is 160nm.
Embodiment 8
A kind of scandium titanate luminescent material, structural formula is In
2sc
2ti
3o
12: 0.01Mn
4+, obtain by the following method:
Take 1mmol respectively, the In of 1mmol, 3mmol, 0.01mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 900 DEG C, calcine 1.5h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 45mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-3pa, underlayer temperature is 250 DEG C, then passes into argon gas, airshed is 10sccm, and under the operating pressure of 0.2Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 60W, depositing time is 25min, after deposition terminates, under 0.09Pa pressure, in argon gas atmosphere, anneal 1 hour at the temperature of 500 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is In
2sc
2ti
3o
12: 0.01Mn
4+, be light-emitting film, light-emitting film thickness is 55nm.
Embodiment 9
A kind of scandium titanate luminescent material, structural formula is In
2sc
2ti
3o
12: 0.05Mn
4+, obtain by the following method:
Take 1mmol respectively, the In of 1mmol, 3mmol, 0.05mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 1300 DEG C, calcine 1.5h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 95mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-5pa, underlayer temperature is 750 DEG C, then passes into argon gas, airshed is 35sccm, and under the operating pressure of 4Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 150W, depositing time is 20min, after deposition terminates, under 0.01Pa pressure, in argon gas atmosphere, anneal 3 hours at the temperature of 800 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is In
2sc
2ti
3o
12: 0.05Mn
4+, be light-emitting film, light-emitting film thickness is 330nm.
Embodiment 10
A kind of scandium titanate luminescent material, structural formula is Tl
2sc
2ti
3o
12: 0.03Mn
4+, obtain by the following method:
Take 1mmol respectively, the Tl of 1mmol, 3mmol, 0.03mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 1250 DEG C, calcine 2h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 60mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 5.0 × 10
-4pa, underlayer temperature is 500 DEG C, then passes into argon gas, airshed is 25sccm, and under the operating pressure of 2Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 180W, depositing time is 30min, after deposition terminates, under 0.08Pa pressure, in argon gas atmosphere, anneal 2 hours at the temperature of 600 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is Tl
2sc
2ti
3o
12: 0.03Mn
4+, be light-emitting film, light-emitting film thickness is 150nm.
Embodiment 11
A kind of scandium titanate luminescent material, structural formula is Tl
2sc
2ti
3o
12: 0.01Mn
4+, obtain by the following method:
Take 1mmol respectively, the Tl of 1mmol, 3mmol, 0.01mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 900 DEG C, calcine 1h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 45mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-3pa, underlayer temperature is 250 DEG C, then passes into argon gas, airshed is 10sccm, and under the operating pressure of 0.2Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 70W, depositing time is 15min, after deposition terminates, under 0.006Pa pressure, in argon gas atmosphere, anneal 1 hour at the temperature of 500 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is Tl
2sc
2ti
3o
12: 0.01Mn
4+, be light-emitting film, light-emitting film thickness is 60nm.
Embodiment 12
A kind of scandium titanate luminescent material, structural formula is Tl
2sc
2ti
3o
12: 0.05Mn
4+, obtain by the following method:
Take 1mmol respectively, the Tl of 1mmol, 3mmol, 0.05mmol
2o
3, Sc
2o
3, TiO
2, MnO
2powder;
Insert in roasting assembly after described powder is mixed, at 1300 DEG C, calcine 1.5h, obtain the Bulk ceramic target of Φ 50 × 2mm, and this target is placed in the vacuum film coating chamber of magnetron sputtering equipment;
Get ito glass substrate, priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, and with plasma processor, the vacuum film coating chamber that plasma treatment is placed on magnetron sputtering equipment is carried out to it, the distance arranging described substrate and described ceramic target is 95mm;
With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-5pa, underlayer temperature is 750 DEG C, then passes into argon gas, airshed is 35sccm, and under the operating pressure of 4Pa, the ion bombardment ceramic target adopting magnetron sputtering to produce also deposits, the power of magnetron sputtering is 180W, depositing time is 30min, after deposition terminates, under 0.03Pa pressure, in argon gas atmosphere, anneal 3 hours at the temperature of 800 DEG C, obtain the scandium titanate luminescent material be deposited on substrate, the structural formula of described luminescent material is Tl
2sc
2ti
3o
12: 0.05Mn
4+, be light-emitting film, light-emitting film thickness is 350nm.
Embodiment 13
A kind of membrane electro luminescent device, as shown in Figure 3, the structure of this membrane electro luminescent device is the glass substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 that stack gradually, wherein, anode 2 is ITO transparent conductive film, the material of negative electrode 4 is Ag, and the material of luminescent layer 3 is structural formula obtained in the embodiment of the present invention 1 is Al
2sc
2ti
3o
12: 0.03Mn
4+luminescent material.
Fig. 4 is the voltage of membrane electro luminescent device prepared by the present embodiment and electric current and brightness relationship figure, curve 1 is voltage and current density relation curve in the diagram, can find out that device can find out device luminescence from 6.0V, curve 2 is voltage and brightness relationship curve, and high-high brightness is 190cd/m
2, show that device has the good characteristics of luminescence.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a scandium titanate luminescent material, is characterized in that, structural formula is R
2sc
2ti
3o
12: xMn
4+, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05.
2. scandium titanate luminescent material as claimed in claim 1, it is characterized in that, the value of described x is 0.03.
3. a preparation method for scandium titanate luminescent material, is characterized in that, comprises the following steps:
According to R
2sc
2ti
3o
12: xMn
4+the stoichiometric ratio of each element provides or prepares ceramic target, and wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05;
Substrate and described ceramic target are placed in the vacuum film coating chamber of magnetron sputtering equipment, arranging vacuum tightness is 1.0 × 10
-3~ 1.0 × 10
-5pa, underlayer temperature is 250 ~ 750 DEG C, distance between described substrate and ceramic target is 45 ~ 95mm, pass into 10 ~ 35sccm argon gas, under the pressure of 0.2 ~ 4Pa, adopt the method for magnetron sputtering to deposit over the substrate and obtain scandium titanate luminescent material, wherein, the power of magnetron sputtering is 30 ~ 200W;
The structural formula of described scandium titanate luminescent material is R
2sc
2ti
3o
12: xMn
4+, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05.
4. the preparation method of scandium titanate luminescent material as claimed in claim 3, is characterized in that, described in provide or the step of preparing ceramic target comprises:
R is taken respectively by the mol ratio of 1: 1: 3: x
2o
3, Sc
2o
3, TiO
2, MnO
2powder, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05;
Insert in roasting assembly after the above-mentioned powder taken is mixed, calcine 0.5 ~ 3 hour at 900 ~ 1300 DEG C, obtain Bulk ceramic target.
5. the preparation method of scandium titanate luminescent material as claimed in claim 3, it is characterized in that, describedly obtain in the process of scandium titanate luminescent material at deposited on substrates, comprise the anneal to gained scandium titanate luminescent material, the mode of described anneal is: after deposited on substrates scandium titanate luminescent material, the pressure of adjustment vacuum plating indoor is 0.001 ~ 0.1Pa, under an argon atmosphere, and anneal 1 ~ 3 hour at 500 ~ 800 DEG C.
6. the preparation method of scandium titanate luminescent material as claimed in claim 3, it is characterized in that, the value of described x is 0.03.
7. a membrane electro luminescent device, comprises substrate, anode, luminescent layer and negative electrode, it is characterized in that, the material of described luminescent layer is scandium titanate luminescent material, and the structural formula of described scandium titanate luminescent material is R
2sc
2ti
3o
12: xMn
4+, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05.
8. a preparation method for membrane electro luminescent device, is characterized in that, comprises the following steps:
According to R
2sc
2ti
3o
12: xMn
4+the stoichiometric ratio of each element provides or prepares ceramic target, and wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05;
Substrate and described ceramic target are placed in the vacuum film coating chamber of magnetron sputtering equipment, arranging vacuum tightness is 1.0 × 10
-3~ 1.0 × 10
-5pa, underlayer temperature is 250 ~ 750 DEG C, distance between described substrate and ceramic target is 45 ~ 95mm, pass into 10 ~ 35sccm argon gas, under the pressure of 0.2 ~ 4Pa, adopt the method for magnetron sputtering to deposit over the substrate and obtain scandium titanate luminescent material, wherein, the power of magnetron sputtering is 30 ~ 200W;
The structural formula of described scandium titanate luminescent material is R
2sc
2ti
3o
12: xMn
4+, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05;
Evaporation negative electrode on described scandium titanate luminescent material, obtains membrane electro luminescent device again.
9. the preparation method of membrane electro luminescent device as claimed in claim 8, is characterized in that, described in provide or the step of preparing ceramic target comprises:
R is taken respectively by the mol ratio of 1: 1: 3: x
2o
3, Sc
2o
3, TiO
2, MnO
2powder, wherein, R is Al, Ga, In or Tl, and the span of x is 0.01 ~ 0.05;
Insert in roasting assembly after the above-mentioned powder taken is mixed, calcine 0.5 ~ 3 hour at 900 ~ 1300 DEG C, obtain Bulk ceramic target.
10. the preparation method of membrane electro luminescent device as claimed in claim 8, it is characterized in that, describedly obtain in the process of scandium titanate luminescent material at deposited on substrates, comprise the anneal to gained scandium titanate luminescent material, the mode of described anneal is: after deposited on substrates scandium titanate luminescent material, the pressure of adjustment vacuum plating indoor is 0.001 ~ 0.1Pa, under an argon atmosphere, and anneal 1 ~ 3 hour at 500 ~ 800 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105219387A (en) * | 2015-07-31 | 2016-01-06 | 江苏师范大学 | Metatitanic acid alkali red illuminating material of a kind of additive Mn and its preparation method and application |
| CN106433643A (en) * | 2016-09-29 | 2017-02-22 | 湘潭大学 | Near-infrared titanate fluorescent powder and preparation method thereof |
| CN106701073A (en) * | 2017-01-06 | 2017-05-24 | 江苏师范大学 | Mn4+ ion doped titanate-based red fluorescent powder and preparation method thereof |
| CN116875307A (en) * | 2023-07-19 | 2023-10-13 | 常熟理工学院 | Tetravalent manganese ion activated titanate-based red luminescent material and preparation method thereof |
| CN116875307B (en) * | 2023-07-19 | 2024-05-28 | 常熟理工学院 | Tetravalent manganese ion activated titanate-based red luminescent material and preparation method thereof |
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2013
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105219387A (en) * | 2015-07-31 | 2016-01-06 | 江苏师范大学 | Metatitanic acid alkali red illuminating material of a kind of additive Mn and its preparation method and application |
| CN106433643A (en) * | 2016-09-29 | 2017-02-22 | 湘潭大学 | Near-infrared titanate fluorescent powder and preparation method thereof |
| CN106433643B (en) * | 2016-09-29 | 2018-06-29 | 湘潭大学 | A kind of titanate near-infrared fluorescent powder and preparation method thereof |
| CN106701073A (en) * | 2017-01-06 | 2017-05-24 | 江苏师范大学 | Mn4+ ion doped titanate-based red fluorescent powder and preparation method thereof |
| CN106701073B (en) * | 2017-01-06 | 2018-12-04 | 江苏师范大学 | Mn4+ ion doped titanate-based red fluorescent powder and preparation method thereof |
| CN116875307A (en) * | 2023-07-19 | 2023-10-13 | 常熟理工学院 | Tetravalent manganese ion activated titanate-based red luminescent material and preparation method thereof |
| CN116875307B (en) * | 2023-07-19 | 2024-05-28 | 常熟理工学院 | Tetravalent manganese ion activated titanate-based red luminescent material and preparation method thereof |
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Application publication date: 20150603 |