CN104745180A - Manganese-doped gallate luminescent film and its preparation method and use - Google Patents
Manganese-doped gallate luminescent film and its preparation method and use Download PDFInfo
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Abstract
The invention discloses a manganese-doped gallate luminescent film and its preparation method and use. The film has a general molecular formula of MeGa2-xO4: xMn<2+>, wherein MeGa2O4 is a matrix, Me represents Ca, Sr or Ba, Mn<2+> is an activation element and is used as a main luminescent center of the film, and x is in a range of 0.01-0.08. Through a metal organic chemical vapor deposition method (MOCVD), the manganese-doped gallate luminescent film (MeGa2-xO4: xMn<2+>) producing red lights is prepared, and has a strong luminescent peak at the wave length of 655nm in a film electroluminescent spectra (EL).
Description
Technical field
The present invention relates to light-emitting film preparation field, particularly relate to a kind of additive Mn gallate light-emitting film 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.At present, research colour and extremely panchromatic TFELD, the material of exploitation multiband luminescence is the developing direction of this problem.
In the research of LED fluorescent powder, the fluorescent material of rear-earth-doped gallate matrix, the emmission spectrum that its excitation spectrum can mate existing near ultraviolet LED preferably can obtain good ruddiness exciting to blue light.But, be prepared into electroluminescent film with non-rear-earth-doped gallate as luminescent material, have not yet to see report.
Summary of the invention
Problem to be solved by this invention is to provide a kind of additive Mn gallate light-emitting film that can be applied to as emitting layer material in organic electroluminescence device.
Technical scheme of the present invention is as follows:
A kind of additive Mn gallate light-emitting film, its general structure is MeGa
2-xo
4: xMn
2+; Wherein, MeGa
2o
4be matrix, Me is Ca, Sr or Ba, Mn
2+be active element, serve as main luminescence center in the film; The value of x is 0.01 ~ 0.08; The value of preferred x is 0.05; Wherein, gallate matrix is a kind of common phosphor material powder, and abundant raw material is cheap, and asepsis environment-protecting, has good electricity and optical property, can be in luminescence and provides good crystal field; Ca, Sr, Ba are similar alkali earth metals, and the gallate performance of composition is similar.
The present invention also provides a kind of preparation method of above-mentioned additive Mn gallate light-emitting film, comprises the steps:
(1), priority toluene, acetone and ethanol respectively ultrasonic cleaning substrate (substrate is the ito glass that Nan Bo company buys) 5 minutes, then clean with distilled water flushing, the air-dry rear feeding vacuum coating film equipment reaction chamber of nitrogen;
(2), to vacuum coating film equipment reaction chamber vacuumize process, make its vacuum tightness be evacuated to 1.0 × 10
-2pa ~ 1.0 × 10
-3after Pa; Heat treating substrates 10 ~ 30 minutes at prior to 700 DEG C, then temperature is reduced to 250 DEG C ~ 650 DEG C (preferably 500 DEG C);
(3) rotating machine of filming equipment is opened, regulate coating process parameter: the rotating speed of substrate bracket is 50 ~ 1000 revs/min, first pass into airshed and be 5 ~ 15sccm and the Ar carrier gas containing organometallic sources, then pass into the oxygen that airshed is 10 ~ 200sccm, start the deposition of film; Wherein, described organometallic sources selects mol ratio to be 1:(2-x respectively): the chemical formula of x is (C
5h
5)
2the cyclopentadiene alkaline earth salt of Me, trimethyl-gallium (DMGa) and the luxuriant manganese of methyl two (MCp); Wherein, pass into oxygen as reaction gas, mocvd method prepares the prerequisite of sull;
(4) thickness of film to be deposited is 80 ~ 300nm(preferred thickness is 150nm) after, close the Ar carrier gas containing organometallic sources, and continue logical oxygen, and the temperature of reaction chamber is dropped to room temperature, namely obtaining general structure is MeGa
2-xo
4: xMn
2+additive Mn gallate light-emitting film; Wherein, MeGa
2o
4be matrix, Me is Ca, Sr or Ba, Mn
2+be active element, serve as main luminescence center in the film; The value of x is 0.01 ~ 0.08.
In the preparation method of described additive Mn gallate light-emitting film, preferably, vacuumizing process to vacuum coating film equipment reaction chamber adopts mechanical pump and molecular pump to vacuumize; The vacuum tightness of preferred reaction room is 4.0 × 10
-3pa.
In the preparation method of described additive Mn gallate light-emitting film, preferred coating process parameter: the rotating speed of substrate bracket is 300 revs/min, the airshed of Ar carrier gas is 10sccm, and the airshed of oxygen is 120sccm.
The present invention provides again a kind of above-mentioned additive Mn gallate light-emitting film as the application of organic electroluminescence device luminescent layer film.
The present invention utilizes Metalorganic Chemical Vapor Deposition (MOCVD), prepares ruddiness additive Mn gallate light-emitting film (MeGa
2-xo
4: xMn
2+), obtain in the electroluminescence spectrum (EL) of film, have very strong glow peak in 655nm position, relative luminous intensity is about 2520, can be used as the potential application material of membrane electro luminescent device.
Accompanying drawing explanation
Fig. 1 is the EL spectrogram of the additive Mn gallate light-emitting film that embodiment 8 obtains;
Fig. 2 is the structural representation of the organic electroluminescence device that embodiment 12 obtains.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described
Embodiment 1: substrate is the ito glass bought from Nan Bo company, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.4.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into three kinds of organic source bis-cyclopentadiene magnesium (C
5h
5)
2the carrier gas Ar gas of Mg, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.95:0.05, and pass into oxygen, flow is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film MgGa
1.95o
4: 0.05Mn
2+.
Embodiment 2: substrate is the ito glass bought from Nan Bo company, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.1.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into three kinds of organic source bis-cyclopentadiene magnesium (C
5h
5)
2the carrier gas Ar gas of Mg, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.99:0.01, and pass into oxygen, flow is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film MgGa
1.99o
4: 0.01Mn
2+.
Embodiment 3: substrate is the ito glass bought from Nan Bo company, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.1.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into three kinds of organic source bis-cyclopentadiene magnesium (C
5h
5)
2the carrier gas Ar gas of Mg, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.92:0.08, and pass into oxygen, flow is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film MgGa
1.92o
4: 0.08Mn
2+.
Embodiment 4: substrate is the ito glass bought from Nan Bo company, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.4.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into three kinds of organic source cyclopentadiene calcium (C
5h
5)
2the carrier gas Ar gas of Ca, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.95:0.05, and pass into oxygen, flow is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film CaGa
1.95o
4: 0.05Mn
2+.
Embodiment 5: substrate is the ito glass bought from Nan Bo company, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.1.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into three kinds of organic source cyclopentadiene calcium (C
5h
5)
2the carrier gas Ar gas of Ca, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.99:0.01, and pass into oxygen, flow is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film CaGa
1.99o
4: 0.01Mn
2+.
Embodiment 6: substrate is the ito glass bought from Nan Bo company, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.1.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into three kinds of organic source cyclopentadiene calcium (C
5h
5)
2the carrier gas Ar gas of Ca, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.92:0.08, and pass into oxygen, flow is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film CaGa
1.92o
4: 0.08Mn
2+.
Embodiment 7: substrate is the ito glass bought from Nan Bo company, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.4.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into three kinds of organic source cyclopentadiene strontium (C
5h
5)
2the carrier gas Ar gas of Sr, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.95:0.05, and pass into oxygen, flow is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film SrGa
1.95o
4: 0.05Mn
2+.
Embodiment 8: substrate is the ito glass bought from Nan Bo company, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.1.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into three kinds of organic source cyclopentadiene strontium (C
5h
5)
2the carrier gas Ar gas of Sr, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.99:0.01, and pass into oxygen, flow is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film SrGa
1.99o
4: 0.01Mn
2+.
Fig. 1 is the EL spectrogram of the additive Mn gallate light-emitting film that embodiment 8 obtains; As shown in Figure 1, in the electroluminescence spectrum (EL) of the additive Mn gallate light-emitting film that the present embodiment obtains, have very strong glow peak in 655nm position, relative luminous intensity is about 2520, can be used as the potential application material of membrane electro luminescent device.
Embodiment 9: substrate is the ito glass bought from Nan Bo company, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.1.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into three kinds of organic source cyclopentadiene strontium (C
5h
5)
2the carrier gas Ar gas of Sr, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.92:0.08, and pass into oxygen, flow is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film SrGa
1.92o
4: 0.08Mn
2+.
Embodiment 10: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.4.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into three kinds of organic source cyclopentadiene barium (C
5h
5)
2the carrier gas Ar gas of Ba, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.95:0.05, and pass into oxygen, flow is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film BaGa
1.95o
4: 0.05Mn
2+.
Embodiment 11: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.1.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into three kinds of organic source cyclopentadiene barium (C
5h
5)
2the carrier gas Ar gas of Ba, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.99:0.01, and pass into oxygen, flow is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film BaGa
1.99o
4: 0.01Mn
2+.
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 additive Mn gallate light-emitting film.
The preparation process of this organic electroluminescence device is as follows:
Substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.1.0 × 10 are evacuated to by the vacuum tightness of mechanical pump and molecular pump cavity
-2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into three kinds of organic source cyclopentadiene barium (C
5h
5)
2the carrier gas Ar gas of Ba, trimethyl-gallium DMGa and the luxuriant manganese of methyl two (MCp), flow is 10sccm.Wherein, the molar flow of three provenances is than being 1:1.92:0.08, and pass into oxygen, flow is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out additive Mn gallate light-emitting film BaGa
1.92o
4: 0.08Mn
2+.Finally 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 (8)
1. an additive Mn gallate light-emitting film, is characterized in that, its general structure is MeGa
2-xo
4: xMn
2+; Wherein, MeGa
2o
4be matrix, Me is Ca, Sr or Ba, Mn
2+be active element, serve as main luminescence center in the film; The value of x is 0.01 ~ 0.08.
2. additive Mn gallate light-emitting film according to claim 1, is characterized in that, the value of x is 0.05.
3. a preparation method for additive Mn gallate light-emitting film according to claim 1, is characterized in that, comprise the steps:
(1) toluene, acetone and ethanol difference ultrasonic cleaning substrate 5 minutes, are successively used, then clean with distilled water flushing, the air-dry rear feeding vacuum coating film equipment reaction chamber of nitrogen;
(2), to vacuum coating film equipment reaction chamber vacuumize process, make its vacuum tightness be evacuated to 1.0 × 10
-2pa ~ 1.0 × 10
-3after Pa; Heat treating substrates 10 ~ 30 minutes at prior to 700 DEG C, then temperature reduces to 250 DEG C ~ 650 DEG C;
(3) rotating machine of filming equipment is opened, regulate coating process parameter: the rotating speed of substrate bracket is 50 ~ 1000 revs/min, first pass into airshed and be 5 ~ 15sccm and the Ar carrier gas containing organometallic sources, then pass into the oxygen that airshed is 10 ~ 200sccm, start the deposition of film; Wherein, described organometallic sources selects mol ratio to be 1:(2-x respectively): the chemical formula of x is (C
5h
5)
2the cyclopentadiene alkaline earth salt of Me, trimethyl-gallium and the luxuriant manganese of methyl two;
(4) thickness of film to be deposited is after 80 ~ 300nm, closes the Ar carrier gas containing organometallic sources, and continues logical oxygen, and the temperature of reaction chamber is dropped to room temperature, and namely obtaining general structure is MeGa
2-xo
4: xMn
2+additive Mn gallate light-emitting film; Wherein, MeGa
2o
4be matrix, Me is Ca, Sr or Ba, Mn
2+be active element, serve as main luminescence center in the film; The value of x is 0.01 ~ 0.08.
4. the preparation method of additive Mn gallate light-emitting film according to claim 3, is characterized in that, vacuumizes process adopt mechanical pump and molecular pump to vacuumize to vacuum coating film equipment reaction chamber.
5. the preparation method of the additive Mn gallate light-emitting film according to claim 3 or 4, is characterized in that, the vacuum tightness of reaction chamber is 4.0 × 10
-3pa.
6. the preparation method of additive Mn gallate light-emitting film according to claim 3, is characterized in that, coating process parameter: the rotating speed of substrate bracket is 300 revs/min, and the airshed of Ar carrier gas is 10sccm, and the airshed of oxygen is 120sccm.
7. the preparation method of additive Mn gallate light-emitting film according to claim 3, is characterized in that, MeGa
2-xo
4: xMn
2+in the value of x be 0.05.
8. one kind as claimed in claim 1 or 2 additive Mn gallate light-emitting film as the application of organic electroluminescence device luminescent layer film.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106118638A (en) * | 2016-06-13 | 2016-11-16 | 郑甘裕 | A kind of additive Mn gallate luminous material, preparation method and applications |
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2013
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106118638A (en) * | 2016-06-13 | 2016-11-16 | 郑甘裕 | A kind of additive Mn gallate luminous material, preparation method and applications |
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