CN104140812A - III-group scandium silicate luminescent material co-doped with titanium and manganese, preparing method thereof and applications of the material - Google Patents

Abstract

A III-group scandium silicate luminescent material co-doped with titanium and manganese is provided. The chemical formula of the material is Me<3>Sc<2>Si<3>O<12>:xTi<4+>, yMn<4+>, wherein the x is 0.01-0.05, the y is 0.005-0.03, and the Me is aluminum ion, gallium ion, indium ion or thallium ion. In an electroluminescence (EL) spectrum of a luminescent film prepared from the material, strong luminescent peaks exist in the wave length zone of 520 nm. The luminescent film can be used in thin-film electroluminescence displayers. The invention also provides a preparing method of the material and applications of the material.

Description

Tai Meng codope three races scandium silicate luminescent material, preparation method and application thereof

[technical field]

The present invention relates to a kind of Tai Meng codope three races scandium silicate luminescent material, its preparation method, Tai Meng codope three races scandium silicate light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof.

[background technology]

Thin-film electroluminescent displays (TFELD), due to its active illuminating, total solids, the advantage such as shock-resistant, reaction is fast, visual angle is large, Applicable temperature is wide, operation is simple, has caused and paid close attention to widely, and development rapidly.At present, research colour and extremely panchromatic TFELD, the luminous material of exploitation multiband, is the developing direction of this problem.But, can be applicable to the Tai Meng codope three races scandium silicate luminescent material of thin-film electroluminescent displays, have not yet to see report.

[summary of the invention]

Based on this, be necessary to provide membrane electro luminescent device of a kind of Tai Meng codope three races scandium silicate luminescent material that can be applicable to membrane electro luminescent device, its preparation method, Tai Meng codope three races scandium silicate light-emitting film, its preparation method, use Gai Taimeng codope three races scandium silicate luminescent material and preparation method thereof.

One Tai Meng codope three races scandium silicate luminescent material, its chemical formula is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion.

A preparation method for Tai Meng codope three races scandium silicate luminescent material, comprises the following steps:

According to Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺the stoichiometric ratio of each element takes Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂powder also mixes, and wherein, x is that 0.01～0.05, y is 0.005～0.03; And

The powder mixing sintering at 900 DEG C～1300 DEG C is obtained to chemical formula for 0.5 hour～5 hours is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺tai Meng codope three races scandium silicate luminescent material, Me is aluminum ion, gallium ion, indium ion or thallium ion.

One Tai Meng codope three races scandium silicate light-emitting film, the chemical general formula of the material of Gai Taimeng codope three races scandium silicate light-emitting film is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion.

A preparation method for Tai Meng codope three races scandium silicate light-emitting film, comprises the following steps:

According to Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺the stoichiometric ratio of each element takes Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂powder also mixes sintering at 900 DEG C～1300 DEG C and makes target in 0.5 hour～5 hours, and wherein, x is that 0.01～0.05, y is 0.005～0.03;

Described target and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 × 10 ^-3pa～1.0 × 10 ^-5pa; And

Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, laser energy is 50W～500W, is then filmed, and obtaining chemical formula is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺tai Meng codope three races scandium silicate light-emitting film, Me is aluminum ion, gallium ion, indium ion or thallium ion.

The vacuum tightness of described vacuum cavity is 5.0 × 10 ^-4pa, base target spacing is 60mm, and magnetron sputtering operating pressure is 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C, and laser energy is 300W.

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 Tai Meng codope three races scandium silicate luminescent material, and the chemical formula of Gai Taimeng codope three races scandium silicate luminescent material is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion.

A preparation method for membrane electro luminescent device, comprises the following steps:

The substrate with anode is provided;

On described anode, form luminescent layer, the material of described luminescent layer is Tai Meng codope three races scandium silicate luminescent material, and the chemical formula of Gai Taimeng codope three races scandium silicate luminescent material is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion;

On described luminescent layer, form negative electrode.

The preparation of described luminescent layer comprises the following steps:

According to Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺the stoichiometric ratio of each element takes Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂powder also mixes sintering at 900 DEG C～1300 DEG C and makes target in 0.5 hour～5 hours, and wherein, x is that 0.01～0.05, y is 0.005～0.03;

Described target and described substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 × 10 ^-3pa～1.0 × 10 ^-5pa;

Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, laser energy is 50W～500W, is then filmed, and obtaining chemical formula is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺tai Meng codope three races scandium silicate light-emitting film, on described anode, form luminescent layer.

The above-mentioned Tai Meng codope scandium silicate luminescent material (Me of three races ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺) in the electroluminescent spectrum (EL) of the light-emitting film made, there is very strong glow peak in 520nm wavelength zone, can be applied in thin-film electroluminescent displays.

[brief description of the drawings]

Fig. 1 is the structural representation of the membrane electro luminescent device of an embodiment;

Fig. 2 is the electroluminescent spectrogram of the Tai Meng codope three races scandium silicate light-emitting film prepared of embodiment 1;

Fig. 3 is the XRD figure of the Tai Meng codope three races scandium silicate light-emitting film prepared of embodiment 1;

Fig. 4 is the graph of relation between voltage and current density and voltage and the brightness of the membrane electro luminescent device prepared of embodiment 1.

[embodiment]

Below in conjunction with the drawings and specific embodiments, Tai Meng codope three races scandium silicate luminescent material, its preparation method, Tai Meng codope three races scandium silicate light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof are further illustrated.

The Tai Meng codope three races scandium silicate luminescent material of one embodiment, its chemical formula is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion.

Preferably, x is that 0.03, y is 0.01.

Me in Gai Taimeng codope three races scandium silicate luminescent material ₃sc ₂si ₃o ₁₂be matrix, titanium ion and mn ion are active elements.In the electroluminescent spectrum (EL) of the light-emitting film that Gai Taimeng codope three races scandium silicate luminescent material is made, there is very strong glow peak in 520nm wavelength zone, can be applied in thin-film electroluminescent displays.

The preparation method of above-mentioned Tai Meng codope three races scandium silicate luminescent material, comprises the following steps:

Step S11, according to Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺the stoichiometric ratio of each element takes Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂powder, wherein, x is that 0.01～0.05, y is 0.005～0.03.

In this step, preferred, x is that 0.03, y is 0.01.

In this step, preferred, Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂the mol ratio of powder is 3:2:3:(:0.01～0.05): (0.005～0.01);

Step S12, by mix equal powder sintering at 900 DEG C～1300 DEG C within 0.5 hour～5 hours, can obtain Tai Meng codope three races scandium silicate luminescent material, its chemical formula is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion.

In this step, preferably sintering 3 hours at 1250 DEG C.

The Tai Meng codope three races scandium silicate light-emitting film of one embodiment, the chemical general formula of the material of Gai Taimeng codope three races scandium silicate light-emitting film is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺tai Meng codope three races scandium silicate luminescent material, Me is aluminum ion, gallium ion, indium ion or thallium ion.

Preferably, x is that 0.03, y is 0.01.

The preparation method of above-mentioned Tai Meng codope three races scandium silicate light-emitting film, comprises the following steps:

Step S21, press Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺the stoichiometric ratio of each element takes Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂powder also mixes sintering at 900 DEG C～1300 DEG C and makes target in 0.5 hour～5 hours, and wherein, x is that 0.01～0.05, y is 0.005～0.03.

In this step, preferred, x is that 0.03, y is 0.01, and at 1250 DEG C, 3 hours one-tenth diameters of sintering are 50mm, the ceramic target that thickness is 2mm.

Step S22, the target obtaining in step S21 and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 × 10 ^-3pa～1.0 × 10 ^-5pa.

In this step, preferred, vacuum tightness is 5 × 10 ^-4pa.

Step S23, adjustment magnetron sputtering plating processing parameter are: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C; Laser energy is 50W～500W, is then filmed, and obtaining chemical formula is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺tai Meng codope three races scandium silicate light-emitting film, Me is zine ion, magnesium ion, calcium ion, strontium ion or barium ion.

In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C, and laser energy is 300W.

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 Tai Meng codope three races scandium silicate luminescent material, and the chemical formula of Gai Taimeng codope three races scandium silicate luminescent material is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion.The material of negative electrode 4 is silver (Ag).

The preparation method of above-mentioned membrane electro luminescent device, comprises the following steps:

Step S31, 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.The substrate 1 with anode 2 is successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning and use it is carried out to oxygen plasma treatment.

Step S32, on anode 2, form luminescent layer 3, the material of luminescent layer 3 is Tai Meng codope three races scandium silicate luminescent material, and the chemical formula of Gai Taimeng codope three races scandium silicate luminescent material is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion.

In present embodiment, luminescent layer 3 is made by following steps:

First, by Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺the stoichiometric ratio of each element takes Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂powder also mixes sintering at 900 DEG C～1300 DEG C and makes target in 0.5 hour～5 hours, and wherein, x is that 0.01～0.05, y is 0.005～0.03.

In this step, preferred, Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂the mol ratio of powder is 3:2:3:(:0.01～0.05): (0.005～0.01);

In this step, preferred, x is that 0.03, y is 0.01, and at 1250 DEG C, 3 hours one-tenth diameters of sintering are 50mm, the ceramic target that thickness is 2mm.

Secondly, target and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 × 10 ^-3pa～1.0 × 10 ^-5pa.

In this step, preferred, vacuum tightness is 5 × 10 ^-4pa.

Then, adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, laser energy is 50W～500W, is then filmed, and forms luminescent layer 3 on anode 2.

In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C, and laser energy is 300W.

Step S33, 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

Selecting purity is 99.99% powder, by the Al of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.03mmol ₂with 0.01mmol MnO ₂powder, after even mixing, at 1250 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 60mm.The vacuum tightness of cavity is extracted into 5.0 × 10 with mechanical pump and molecular pump ^-4pa, the working gas flow of oxygen is 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 DEG C, laser energy 300W.The sample chemical formula obtaining is Al ₃sc ₂si ₃o ₁₂: 0.03Ti ⁴⁺, 0.01Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

The chemical general formula of the Tai Meng codope three races scandium silicate light-emitting film obtaining in the present embodiment is Al ₃sc ₂si ₃o ₁₂: 0.03Ti ⁴⁺, 0.01Mn ⁴⁺, wherein Al ₃sc ₂si ₃o ₁₂matrix, Ti ⁴⁺and Mn ⁴⁺it is active element.

Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the Tai Meng codope three races scandium silicate light-emitting film obtaining.As seen from Figure 2, in electroluminescence spectrum, there is very strong glow peak in 520nm wavelength zone, can be applied in thin-film electroluminescent displays.

Refer to Fig. 3, Fig. 3 is the XRD curve of the Tai Meng codope three races scandium silicate light-emitting film prepared of embodiment 1, test comparison standard P DF card.As can be seen from Figure 3, diffraction peak is depicted as the peak crystallization of three races's scandium silicate, does not occur the diffraction peak of doped element and other impurity, illustrates that the product that this preparation method obtains has good crystalline quality.

Refer to Fig. 4, Fig. 4 is the graph of relation between voltage and current density and voltage and the brightness of the membrane electro luminescent device prepared of embodiment 1, curve 1 is voltage and current density relation curve, can find out that this device starts luminous from voltage 5.0V, curve 2 is voltage and brightness relationship curve, and the high-high brightness that can find out this device is 77cd/m ², show that device has the good characteristics of luminescence.

Embodiment 2

Selecting purity is 99.99% powder, by the Al of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.01mmol ₂with 0.005mmol MnO ₂powder, after even mixing, at 900 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump ^-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, laser energy 80W.The chemical formula of the sample obtaining is Al ₃sc ₂si ₃o ₁₂: 0.01Ti ⁴⁺, 0.005Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

Embodiment 3

Selecting purity is 99.99% powder, by the Al of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.05mmol ₂with 0.03mmol MnO ₂powder, after even mixing, at 1300 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump ^-5pa, the working gas flow of oxygen is 40sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, laser energy 50W.The chemical formula of the sample obtaining is Al ₃sc ₂si ₃o ₁₂: 0.05Ti ⁴⁺, 0.03Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

Embodiment 4

Selecting purity is 99.99% powder, by the Ga of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.03mmol ₂with 0.01mmol MnO ₂powder, after even mixing, at 1250 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 60mm.The vacuum tightness of cavity is extracted into 5.0 × 10 with mechanical pump and molecular pump ^-4pa, the working gas flow of oxygen is 20sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, laser energy 300W.The chemical formula of the sample obtaining is Ga ₃sc ₂si ₃o ₁₂: 0.03Ti ⁴⁺, 0.01Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

Embodiment 5

Selecting purity is 99.99% powder, by the Ga of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.01mmol ₂with 0.005mmol MnO ₂powder, after even mixing, at 900 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump ^-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C, laser energy 500W.The chemical formula of the sample obtaining is Ga ₃sc ₂si ₃o ₁₂: 0.005Ti ⁴⁺, 0.005Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

Embodiment 6

Selecting purity is 99.99% powder, by the Ga of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.05mmol ₂with 0.03mmol MnO ₂powder, after even mixing, at 1300 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump ^-5pa, the working gas flow of oxygen is 40sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, laser energy 50W.The chemical formula of the sample obtaining is Ga ₃sc ₂si ₃o ₁₂: 0.05Ti ⁴⁺, 0.03Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

Embodiment 7

Selecting purity is 99.99% powder, by the In of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.03mmol ₂with 0.01mmol MnO ₂powder, after even mixing, at 1250 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 60mm.The vacuum tightness of cavity is extracted into 5.0 × 10 with mechanical pump and molecular pump ^-4pa, the working gas flow of oxygen is 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 DEG C, laser energy 150W.The chemical general formula of the sample obtaining is In ₃sc ₂si ₃o ₁₂: 0.03Ti ⁴⁺, 0.01Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

Embodiment 8

Selecting purity is 99.99% powder, by the In of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.01mmol ₂with 0.005mmol MnO ₂powder, after even mixing, at 900 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump ^-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, laser energy 500W.The chemical formula of the sample obtaining is In ₃sc ₂si ₃o ₁₂: 0.01Ti ⁴⁺, 0.005Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

Embodiment 9

Selecting purity is 99.99% powder, by the In of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.05mmol ₂with 0.03mmol MnO ₂powder, after even mixing, at 1300 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump ^-5pa, the working gas flow of oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, laser energy 50W.The chemical formula of the sample obtaining is In ₃sc ₂si ₃o ₁₂: 0.05Ti ⁴⁺, 0.03Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

Embodiment 10

Selecting purity is 99.99% powder, by the Tl of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.03mmol ₂with 0.01mmol MnO ₂powder, after even mixing, at 1250 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 60mm.The vacuum tightness of cavity is extracted into 5.0 × 10 with mechanical pump and molecular pump ^-4pa, the working gas flow of oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, laser energy 300W.The chemical formula of the sample obtaining is Tl ₃sc ₂si ₃o ₁₂: 0.03Ti ⁴⁺, 0.01Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

Embodiment 11

Selecting purity is 99.99% powder, by the Tl of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.01mmol ₂with 0.005mmol MnO ₂powder, after even mixing, at 900 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump ^-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C, laser energy 500W.The chemical formula of the sample obtaining is Tl ₃sc ₂si ₃o ₁₂: 0.01Ti ⁴⁺, 0.005Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

Embodiment 12

Selecting purity is 99.99% powder, by the Tl of 3mmol ₂o ₃, the Sc of 2mmol ₂o ₃, the SiO of 3mmol, the TiO of 0.05mmol ₂with 0.03mmol MnO ₂powder, after even mixing, at 1300 DEG C, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump ^-5pa, the working gas flow of oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, laser energy 50W.The chemical formula of the sample obtaining is Tl ₃sc ₂si ₃o ₁₂: 0.05Ti ⁴⁺, 0.03Mn ⁴⁺light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.

The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (9)

1. a Zhong Taimeng codope three races scandium silicate luminescent material, is characterized in that: its chemical formula is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion.

2. the preparation method of a Zhong Taimeng codope three races scandium silicate luminescent material, is characterized in that, comprises the following steps:

According to Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺the stoichiometric ratio of each element takes Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂powder also mixes, and wherein, x is that 0.01～0.05, y is 0.005～0.03; And

The powder mixing sintering at 900 DEG C～1300 DEG C is obtained to chemical formula for 0.5 hour～5 hours is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺tai Meng codope three races scandium silicate luminescent material, Me is aluminum ion, gallium ion, indium ion or thallium ion.

3. a Zhong Taimeng codope three races scandium silicate light-emitting film, is characterized in that, the chemical general formula of the material of Gai Taimeng codope three races scandium silicate light-emitting film is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion.

4. the preparation method of a Zhong Taimeng codope three races scandium silicate light-emitting film, is characterized in that, comprises the following steps:

According to Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺the stoichiometric ratio of each element takes Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂powder also mixes sintering at 900 DEG C～1300 DEG C and makes target in 0.5 hour～5 hours, and wherein, x is that 0.01～0.05, y is 0.005～0.03;

Described target and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 × 10 ^-3pa～1.0 × 10 ^-5pa; And

Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, laser energy is 50W～500W, is then filmed, and obtaining chemical formula is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺tai Meng codope three races scandium silicate light-emitting film, Me is aluminum ion, gallium ion, indium ion or thallium ion.

5. the preparation method of Tai Meng codope according to claim 4 three races scandium silicate light-emitting film, is characterized in that, the vacuum tightness of described vacuum cavity is 5.0 × 10 ^-4pa, base target spacing is 60mm, and magnetron sputtering operating pressure is 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C, and laser energy is 300W.

6. 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 Tai Meng codope three races scandium silicate luminescent material, and the chemical formula of Gai Taimeng codope three races scandium silicate luminescent material is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion.

7. a preparation method for membrane electro luminescent device, is characterized in that, comprises the following steps:

The substrate with anode is provided;

On described anode, form luminescent layer, the material of described luminescent layer is Tai Meng codope three races scandium silicate luminescent material, and the chemical formula of Gai Taimeng codope three races scandium silicate luminescent material is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺, wherein, x is that 0.01～0.05, y is that 0.005～0.03, Me is aluminum ion, gallium ion, indium ion or thallium ion;

On described luminescent layer, form negative electrode.

8. the preparation method of membrane electro luminescent device according to claim 7, is characterized in that, the preparation of described luminescent layer comprises the following steps:

According to Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺the stoichiometric ratio of each element takes Me ₂o ₃, Sc ₂o ₃, SiO, TiO ₂and MnO ₂powder also mixes sintering at 900 DEG C～1300 DEG C and makes target in 0.5 hour～5 hours, and wherein, x is that 0.01～0.05, y is 0.005～0.03;

Described target and described substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 × 10 ^-3pa～1.0 × 10 ^-5pa;

Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, laser energy is 50W～500W, is then filmed, and obtaining chemical formula is Me ₃sc ₂si ₃o ₁₂: xTi ⁴⁺, yMn ⁴⁺tai Meng codope three races scandium silicate light-emitting film, on described anode, form luminescent layer.

9. the preparation method of membrane electro luminescent device according to claim 8, is characterized in that, described x is that 0.03, y is 0.01.