CN104745184A - Manganese-chromium-codoped zirconium arsenate luminescent film and its preparation method and use - Google Patents
Manganese-chromium-codoped zirconium arsenate luminescent film and its preparation method and use Download PDFInfo
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- CN104745184A CN104745184A CN201310731222.6A CN201310731222A CN104745184A CN 104745184 A CN104745184 A CN 104745184A CN 201310731222 A CN201310731222 A CN 201310731222A CN 104745184 A CN104745184 A CN 104745184A
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- codoped zirconium
- manganese chromium
- zirconium arsenate
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- DJHGAFSJWGLOIV-UHFFFAOYSA-K Arsenate3- Chemical compound [O-][As]([O-])([O-])=O DJHGAFSJWGLOIV-UHFFFAOYSA-K 0.000 title claims abstract description 38
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229940000489 arsenate Drugs 0.000 title claims abstract description 38
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 5
- QDLZHJXUBZCCAD-UHFFFAOYSA-N [Cr].[Mn] Chemical compound [Cr].[Mn] QDLZHJXUBZCCAD-UHFFFAOYSA-N 0.000 claims description 34
- 239000007789 gas Substances 0.000 claims description 33
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 30
- 239000000758 substrate Substances 0.000 claims description 27
- 239000000919 ceramic Substances 0.000 claims description 19
- 239000011651 chromium Substances 0.000 claims description 18
- 238000000137 annealing Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- 238000005401 electroluminescence Methods 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 5
- 239000011572 manganese Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 3
- 238000001228 spectrum Methods 0.000 abstract description 3
- 230000004913 activation Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 33
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 24
- 239000011521 glass Substances 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 229960000935 dehydrated alcohol Drugs 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 238000009832 plasma treatment Methods 0.000 description 12
- 238000004506 ultrasonic cleaning Methods 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000001194 electroluminescence spectrum Methods 0.000 description 6
- 229910017702 MgZr Inorganic materials 0.000 description 3
- 239000012528 membrane Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Landscapes
- Luminescent Compositions (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
The invention discloses a manganese-chromium-codoped zirconium arsenate luminescent film and its preparation method and use. The film has a general molecular formula of RZr4-x-yAs6O24: xMn<4+>, yCr<3+>, wherein RZr4As6O24 is a matrix, Mn<4+> and Cr<3+> are activation elements and are used as main luminescent centers of the film, R represents Mg, Ca, Ba or Sr, x is in a range of 0.01-0.05 and y is in a range of 0.005-0.03. Through a magnetron sputtering device, the manganese-chromium-codoped zirconium arsenate luminescent film (RZr4-x-yAs6O24: xMn<4+>, yCr<3+>) is prepared, has strong luminescent peaks at the wave length of 632nm and 673nm in a film electroluminescent spectra (EL) and can be used as a latent material for a film electroluminescent device.
Description
Technical field
The present invention relates to a kind of light-emitting film material field, particularly relate to a kind of manganese chromium codoped zirconium arsenate and its preparation method and application.
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.
Zirconium arsenate luminescent material is the popular research material as LED fluorescent powder.Burst of ultraviolel blue colour fluorescent powder can as the product of commercialization, and constantly improve in research and development.
Summary of the invention
Goal of the invention is the light-emitting film preparing a kind of manganese chromium codoped zirconium arsenate that can be commercial.
Technical scheme of the present invention is as follows:
A kind of manganese chromium codoped zirconium arsenate light-emitting film provided by the invention, its general structure is RZr
4-x-yas
6o
24: xMn
4+, yCr
3+; Wherein, RZr
4as
6o
24matrix, Mn
4+and Cr
3+be active element, serve as main luminescence center in the film; R is Mg, Ca, Ba or Sr, and the value of x is the value of 0.01 ~ 0.05, y is 0.005 ~ 0.03.
The invention is characterized in and utilize magnetron sputtering equipment, prepare manganese chromium codoped zirconium arsenate RZr
4-x-ysb
6o
24: xEu
2+, yTb
3+light-emitting film.The preparation of film includes several step below:
(1) preparation of ceramic target: take RO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, its mol ratio is 1:(4-x-y): 3:x/2:y/4, after Homogeneous phase mixing, sinters, preferably 1250 DEG C, makes the ceramic target of Φ 50 × 2mm at 900 ~ 1300 DEG C.
(2) ceramic target in step (1) and ITO substrate are loaded the cavity of filming equipment, with mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-3pa ~ 1.0 × 10
-5pa, preferably 5.0 × 10
-4pa;
(3) filming technology parameter is regulated: base target spacing is 45 ~ 95mm, preferred 60mm, and underlayer temperature is 250 DEG C ~ 750 DEG C, preferably 500 DEG C, operating pressure 0.2 ~ 4Pa, preferred 2.0Pa, then pass into argon gas as working gas, gas flow 10 ~ 35sccm, preferred 25sccm, is filmed;
(4) stop masking, the sample obtained is annealed 1 ~ 3h, preferred 2h in 0.01Pa vacuum oven, and annealing temperature is 500 DEG C ~ 800 DEG C, preferably 600 DEG C, and obtain described manganese chromium codoped zirconium arsenate light-emitting film, the general structure of this light-emitting film is RZr
4-x-yas
6o
24: xMn
4+, yCr
3+; Wherein, RZr
4as
6o
24matrix, Mn
4+and Cr
3+be active element, serve as main luminescence center in the film; R is Mg, Ca, Ba or Sr, and the value of x is the value of 0.01 ~ 0.05, y is 0.005 ~ 0.03.
The present invention provides again the application of a kind of above-mentioned manganese chromium codoped zirconium arsenate light-emitting film in organic electroluminescence device luminescent layer field.
The present invention adopts magnetron sputtering equipment, prepares manganese chromium codoped zirconium arsenate light-emitting film RZr
4-x-yas
6o
24: xMn
4+, yCr
3+, obtain in the electroluminescence spectrum (EL) of film, have very strong glow peak in 632nm and 673nm position, relative luminous intensity is respectively 2050 and 2500, can be used as the potential application material of membrane electro luminescent device.
Accompanying drawing explanation
Fig. 1 is the EL luminous spectrum of the manganese chromium codoped zirconium arsenate light-emitting film that embodiment 1 obtains;
Fig. 2 is the structural representation that embodiment 12 obtains organic electroluminescence device.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1: select MgO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.96mmol, 3mmol, 0.015mmol, 0.0025mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 1250 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 5.0 × 10
-4pa, the working gas flow of argon gas is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C.The sample obtained is annealed 2h in 0.01Pa vacuum oven, and annealing temperature is 600 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film MgZr
3.96as
6o
24: 0.03Mn4
+, 0.01Cr
3+.
Fig. 1 is the EL luminous spectrum of the manganese chromium codoped zirconium arsenate light-emitting film that embodiment 1 obtains; As shown in Figure 1, in the electroluminescence spectrum (EL) of manganese chromium codoped zirconium arsenate light-emitting film, have very strong glow peak in 632nm and 673nm position, relative luminous intensity is respectively 2050 and 2500, can be used as the potential application material of membrane electro luminescent device.
Embodiment 2: select MgO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.985mmol, 3mmol, 0.005mmol, 0.00125mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 900 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 1.0 × 10
-3pa, the working gas flow of argon gas is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C.The sample obtained is annealed 1h in 0.01Pa vacuum oven, and annealing temperature is 500 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film MgZr
3.985as
6o
24: 0.01Mn4
+, 0.005Cr
3+.
Embodiment 3: select MgO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.92mmol, 3mmol, 0.025mmol, 0.0075mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 1150 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 1.0 × 10
-5pa, the working gas flow of argon gas is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C.The sample obtained is annealed 3h in 0.01Pa vacuum oven, and annealing temperature is 800 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film MgZr
3.92as
6o
24: 0.05Mn4
+, 0.03Cr
3+.
Embodiment 4: select CaO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.96mmol, 3mmol, 0.015mmol, 0.0025mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 1250 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 5.0 × 10
-4pa, the working gas flow of argon gas is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C.The sample obtained is annealed 2h in 0.01Pa vacuum oven, and annealing temperature is 600 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film CaZr
3.96as
6o
24: 0.03Mn4
+, 0.01Cr
3+.
Embodiment 5: select CaO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.985mmol, 3mmol, 0.005mmol, 0.00125mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 900 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 1.0 × 10
-3pa, the working gas flow of argon gas is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C.The sample obtained is annealed 1h in 0.01Pa vacuum oven, and annealing temperature is 500 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film CaZr
3.985as
6o
24: 0.01Mn4
+, 0.005Cr
3+.
Embodiment 6: select CaO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.92mmol, 3mmol, 0.025mmol, 0.0075mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 1150 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 1.0 × 10
-5pa, the working gas flow of argon gas is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C.The sample obtained is annealed 3h in 0.01Pa vacuum oven, and annealing temperature is 800 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film CaZr
3.92as
6o
24: 0.05Mn4
+, 0.03Cr
3+.
Embodiment 7: select SrO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.96mmol, 3mmol, 0.015mmol, 0.0025mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 1250 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 5.0 × 10
-4pa, the working gas flow of argon gas is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C.The sample obtained is annealed 2h in 0.01Pa vacuum oven, and annealing temperature is 600 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film SrZr
3.96as
6o
24: 0.03Mn4
+, 0.01Cr
3+.
Embodiment 8: select SrO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.985mmol, 3mmol, 0.005mmol, 0.00125mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 900 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 1.0 × 10
-3pa, the working gas flow of argon gas is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C.The sample obtained is annealed 1h in 0.01Pa vacuum oven, and annealing temperature is 500 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film SrZr
3.985as
6o
24: 0.01Mn4
+, 0.005Cr
3+.
Embodiment 9: select SrO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.92mmol, 3mmol, 0.025mmol, 0.0075mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 1150 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 1.0 × 10
-5pa, the working gas flow of argon gas is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C.The sample obtained is annealed 3h in 0.01Pa vacuum oven, and annealing temperature is 800 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film SrZr
3.92as
6o
24: 0.05Mn4
+, 0.03Cr
3+.
Embodiment 10: select BaO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.96mmol, 3mmol, 0.015mmol, 0.0025mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 1250 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 5.0 × 10
-4pa, the working gas flow of argon gas is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C.The sample obtained is annealed 2h in 0.01Pa vacuum oven, and annealing temperature is 600 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film BaZr
3.96as
6o
24: 0.03Mn4
+, 0.01Cr
3+.
Embodiment 11: select BaO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.985mmol, 3mmol, 0.005mmol, 0.00125mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 900 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 1.0 × 10
-3pa, the working gas flow of argon gas is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C.The sample obtained is annealed 1h in 0.01Pa vacuum oven, and annealing temperature is 500 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film BaZr
3.985as
6o
24: 0.01Mn4
+, 0.005Cr
3+.
Embodiment 12: the present embodiment is organic electroluminescence device, as shown in Figure 2, its structure comprises glass substrate 1, ITO transparent conductive film 2 as anode, light-emitting film layer 3, Ag layer 4 as negative electrode; Wherein, light-emitting film layer 3 is manganese chromium codoped zirconium arsenate light-emitting film.
The preparation technology of this organic electroluminescence device is as follows:
Select BaO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, 1mmol, 3.92mmol, 3mmol, 0.025mmol, 0.0075mmol, after Homogeneous phase mixing, sinter the ceramic target of Φ 50 × 2mm into, and loaded in vacuum cavity by target at 1150 DEG C.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, 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 tightness of cavity is extracted into 1.0 × 10
-5pa, the working gas flow of argon gas is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C.The sample obtained is annealed 3h in 0.01Pa vacuum oven, and annealing temperature is 800 DEG C.Obtain manganese chromium codoped zirconium arsenate light-emitting film BaZr
3.92as
6o
24: 0.05Mn4
+, 0.03Cr
3+, then evaporation one deck Ag on light-emitting film, as negative electrode, obtained organic electroluminescence device.
Should be understood that, the above-mentioned statement for present pre-ferred embodiments is comparatively detailed, and therefore can not think the restriction to scope of patent protection of the present invention, scope of patent protection of the present invention should be as the criterion with claims.
Claims (9)
1. a manganese chromium codoped zirconium arsenate light-emitting film, is characterized in that, its general structure is RZr
4-x-yas
6o
24: xMn
4+, yCr
3+; Wherein, RZr
4as
6o
24matrix, Mn
4+and Cr
3+be active element, serve as main luminescence center in the film; R is Mg, Ca, Ba or Sr, and the value of x is the value of 0.01 ~ 0.05, y is 0.005 ~ 0.03.
2. manganese chromium codoped zirconium arsenate light-emitting film according to claim 1, is characterized in that, the value of x is the value of 0.03, y is 0.01.
3. a preparation method for manganese chromium codoped zirconium arsenate light-emitting film according to claim 1, is characterized in that, comprise the steps:
(1) preparation of ceramic target: take RO, ZrO
2, As
2o
5, MnO
2and Cr
2o
3powder, its mol ratio is 1:(4-x-y): 3:x/2:y/4, after Homogeneous phase mixing, sinters, makes the ceramic target of Φ 50 × 2mm at 900 ~ 1300 DEG C;
(2) ceramic target in step (1) and ITO substrate are loaded in the vacuum cavity of filming equipment, with mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-3pa ~ 1.0 × 10
-5pa;
(3) filming technology parameter is regulated: base target spacing is 45 ~ 95mm, and underlayer temperature is 250 DEG C ~ 750 DEG C, and then operating pressure 0.2 ~ 4Pa passes into argon gas as working gas, gas flow 10 ~ 35sccm, carry out film preparation;
(4) stop film preparation, the sample obtained is annealed 1 ~ 3h in 0.01Pa vacuum oven, and annealing temperature is 500 DEG C ~ 800 DEG C, and obtain described manganese chromium codoped zirconium arsenate light-emitting film, the general structure of this light-emitting film is RZr
4-x-yas
6o
24: xMn
4+, yCr
3+; Wherein, RZr
4as
6o
24matrix, Mn
4+and Cr
3+be active element, serve as main luminescence center in the film; R is Mg, Ca, Ba or Sr, and the value of x is the value of 0.01 ~ 0.05, y is 0.005 ~ 0.03.
4. the preparation method of manganese chromium codoped zirconium arsenate light-emitting film according to claim 3, it is characterized in that, in the preparation process of ceramic target, sintering temperature is 1250 DEG C.
5. the preparation method of manganese chromium codoped zirconium arsenate light-emitting film according to claim 3, it is characterized in that, the vacuum tightness in filming equipment vacuum cavity is 5.0 × 10
-4pa.
6. the preparation method of manganese chromium codoped zirconium arsenate light-emitting film according to claim 3, is characterized in that, adjustment filming technology parameter is: base target spacing is 60mm, underlayer temperature is 500 DEG C, pass into argon gas as working gas, gas flow is 25sccm, and operating pressure is 2.0Pa.
7. the preparation method of manganese chromium codoped zirconium arsenate light-emitting film according to claim 3, it is characterized in that, the sample obtained annealing time in 0.01Pa vacuum oven is 2h, and annealing temperature is 600 DEG C.
8. the preparation method of manganese chromium codoped zirconium arsenate light-emitting film according to claim 3, is characterized in that, the value of x is the value of 0.03, y is 0.01.
9. the application of manganese chromium codoped zirconium arsenate light-emitting film in organic electroluminescence device luminescent layer field as claimed in claim 1 or 2.
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|---|---|---|---|
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|---|---|---|---|
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ID=53585455
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106147764A (en) * | 2016-06-13 | 2016-11-23 | 郑甘裕 | A kind of manganese-chromium-codoped zirconium arsenate light-emitting film, preparation method and applications |
-
2013
- 2013-12-26 CN CN201310731222.6A patent/CN104745184A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106147764A (en) * | 2016-06-13 | 2016-11-23 | 郑甘裕 | A kind of manganese-chromium-codoped zirconium arsenate light-emitting film, preparation method and applications |
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