CN102796517A - Nitrogenous magnesium silicate film, and preparation method and application thereof - Google Patents
Nitrogenous magnesium silicate film, and preparation method and application thereof Download PDFInfo
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- CN102796517A CN102796517A CN2011101340030A CN201110134003A CN102796517A CN 102796517 A CN102796517 A CN 102796517A CN 2011101340030 A CN2011101340030 A CN 2011101340030A CN 201110134003 A CN201110134003 A CN 201110134003A CN 102796517 A CN102796517 A CN 102796517A
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Abstract
The invention relates to the field of preparation of semiconductor materials, and provides a nitrogenous magnesium silicate film which is a titanium-doped nitrogenous magnesium silicate film of which the general formula is Mg1-XSi2O2N2:XTi4+, wherein X-0.01-0.15. The invention also provides a preparation method of the nitrogenous magnesium silicate film, which comprises the following steps: mixing MgO powder, SiO2 powder, Si3N4 powder and TiO2 powder, and sintering to obtain a target; and filling the target into a magnetron sputtering chamber, vacuumizing, setting working parameters, and sputtering to obtain the nitrogenous magnesium silicate film. The invention also provides application of the nitrogenous magnesium silicate film in electroluminescent devices.
Description
Technical field
The invention belongs to the photoelectric semiconductor material field, be specifically related to a kind of nitrogenous silicic acid magnesium film.
Background technology
Compare with the image display that traditional luminescent powder is made, light-emitting film contrast gradient, resolving power, thermal conduction, homogeneity, and aspects such as the tack of substrate, outgas speed all demonstrate stronger meliority.Therefore, as functional materials, light-emitting film has wide application prospect in such as cathode tube (CRTs), electroluminescent demonstration (ELDs) and FED FPD fields such as (FEDs).
Thin-film electroluminescent displays (TFELD) since its active illuminating, total solidsization, shock-resistant, advantage such as reaction is fast, the visual angle is big, Applicable temperature is wide, operation is simple caused and paid close attention to widely, and development rapidly.Be that the monochromatic TFELD of luminescent layer is full-fledged and realized commercialization with ZnS:Mn.Research is colored to be reached to panchromatic TFELD, and the luminous material of exploitation multiband is extremely urgent task.In the luminescence system material, rare earth ion doped silicates fluorescent material has obtained deep research, can access good ruddiness exciting to blue light.Simultaneously, its chemicalstability and thermostability are improved owing to add an amount of nitride, and the excitation wavelength that can be changed in a big way, therefore, nitrogenous silicate is the substrate material that has potentiality as luminescent material.But, present this type of material powder morphology often of report, and the rare earth price is more expensive, scarcity of resources makes application difficult in actual production, cost is higher.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective of prior art, and a kind of nitrogenous silicic acid magnesium film is provided.
The embodiment of the invention is achieved in that first aspect provides a kind of nitrogenous silicic acid magnesium film, and said film is titanium doped nitrogenous silicic acid magnesium film, and the chemical general formula of said titanium doped nitrogenous silicic acid magnesium film is Mg
1-XSi
2O
2N
2:
XTi
4+, wherein, the span of X is 0.01～0.15.
Another purpose of the embodiment of the invention is to provide the preparation method of above-mentioned nitrogenous silicic acid magnesium film, and it comprises the steps:
With MgO powder, SiO
2Powder, Si
3N
4Powder and TiO
2Powder is according to mol ratio (1-X): 0.5: 0.5: X mixes, and sintering is as target, and wherein, the span of said X is 0.01～0.15;
Said target is packed in the magnetron sputtering cavity; Vacuumize, it is 0.2Pa～4.5Pa that operating pressure is set, and feeds the mixed gas of rare gas element and hydrogen; Mixed gas flow is 15sccm～30sccm; Underlayer temperature is 350 ℃～750 ℃, and sputtering power is 30W～150W, and sputter gets nitrogenous silicic acid magnesium film.
Another purpose of the embodiment of the invention is to provide above-mentioned nitrogenous silicic acid magnesium film in the application in feds, cathode tube and/or electroluminescent device.
The embodiment of the invention provides a kind of nitrogenous silicic acid magnesium film, and through the Ti nitrogenous Magnesium Silicate q-agent that mixes, it is low to obtain cost, thermostability and the stable high electroluminescent film of luminous intensity.The preparation method adopts magnetron sputtering method, and it has the sedimentation rate height, the film tack is good, easy to control and can realize advantages such as big area deposition.Further, this film shows the advantage that stability is high, the life-span is long in the application of electroluminescent device.
Description of drawings
Fig. 1 is preparing method's the schema of the nitrogenous silicic acid magnesium film of the embodiment of the invention;
Fig. 2 is with the nitrogenous silicic acid magnesium film of the embodiment of the invention structural representation as the electroluminescent device of making luminescent layer;
Fig. 3 is the nitrogenous silicic acid magnesium film electroluminescent spectrum figure of the embodiment of the invention 1 preparation;
Fig. 4 be the embodiment of the invention 1 preparation nitrogenous silicic acid magnesium film 300 ℃ use down after, luminous intensity and time relation figure;
Fig. 5 is the X-ray diffractogram of the nitrogenous silicic acid magnesium film of the embodiment of the invention 1 preparation.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is done further explain below in conjunction with accompanying drawing and embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
The embodiment of the invention is achieved in that first aspect provides a kind of nitrogenous silicic acid magnesium film, and said film is titanium doped nitrogenous silicic acid magnesium film, and the chemical general formula of said titanium doped nitrogenous silicic acid magnesium film is Mg
1-XSi
2O
2N
2:
XTi
4+, wherein, the span of X is 0.01～0.15.
Substrate material Mg
1-XSi
2O
2N
2Has the high advantage of chemicalstability and thermostability, an amount of Ti
4+Doping can obtain the titanium doped preferably nitrogenous Magnesium Silicate q-agent of luminous intensity, and preferred, the span of X is 0.02～0.08, can guarantee to obtain thin-film light emitting intensity and crystalline quality preferably this moment.
Another purpose of the embodiment of the invention is to provide the preparation method of the nitrogenous silicic acid magnesium film of the embodiment of the invention, sees also Fig. 1, and it comprises the steps:
S01: with MgO powder, SiO
2Powder, Si
3N
4Powder and TiO
2Powder is according to mol ratio (1-X): 0.5: 0.5: X mixes, and sintering is as target, and wherein, the span of said X is 0.01～0.15;
S02: said target is packed in the magnetron sputtering cavity; Vacuumize, it is 0.2Pa～4.5Pa that operating pressure is set, and feeds the mixed gas of rare gas element and hydrogen; Mixed gas flow is 15sccm～30sccm; Underlayer temperature is 350 ℃～750 ℃, and sputtering power is 30W～150W, and sputter gets nitrogenous silicic acid magnesium film.
Among the step S01, with MgO powder, SiO
2Powder, Si
3N
4Powder and TiO
2Powder is according to mol ratio (1-X): 0.5: 0.5: X mixed, and high temperature sintering for example at 900 ℃～1300 ℃ sintering temperatures, obtains target.Preferably, sintering temperature is 1200 ℃.The purity of above-mentioned powder is preferably greater than 99.99%.The quality that takes by weighing is respectively: MgO 6.8g～7.92g, SiO
26g, Si
3N
414g and TiO
20.16g～2.4g makes the mol ratio of four kinds of powders be (1-X): 0.5: 0.5: X, this moment, the X value was 0.01～0.15; Preferably the X value is 0.06～0.1, TiO
2Quality be 0.9g～1.6g, more preferably the X value is 0.08, TiO
2Quality be 1.28g.The content of matrix composition and alloying element is the important factor that influences film performance and structure.Owing to add an amount of nitride its chemicalstability and thermostability are improved in the substrate material, and the excitation wavelength that can be changed in a big way, and the content of Ti can influence luminous intensity.But doped metal ion is influential to material structure, and external metals ion gets into lattice; Make crystalline structure generation fractional distortion, therefore, doping is excessive; Can cause lattice distortion excessive, upset the ion ordering in the lattice or cause generating in the material dephasign, material property is seriously weakened.
Among the step S02, substrate is hard substrates such as sapphire, silica glass, silicon chip.Use preceding with acetone, absolute ethyl alcohol and deionized water supersound washing.Also can select substrate for use, like the ito glass substrate based on further application.The distance of target and substrate is preferably 50mm～90mm.More preferably, the distance of target and substrate is 70mm.After target is packed in the sputter cavity, the vacuum tightness of cavity is evacuated to 1.0 * 10 with mechanical pump or molecular pump
-3Pa～1.0 * 10
-5More than the Pa, be preferably 6.0 * 10
-4Pa.Obtain the nitrogenous silicic acid magnesium film of excellent performance, processing condition are provided with extremely important.Working gas in the sputtering chamber is the mixed gas of rare gas element and hydrogen, and wherein, the volume percent of hydrogen is 1%～15%, is preferably 3%～8%.Preferably, mixed gas flow is 20sccm～25sccm, and operating pressure is 0.8Pa～2.5Pa, and underlayer temperature is 400 ℃～600 ℃, and sputtering power is 80W～120W.Further, the nitrogenous silicic acid magnesium film that makes is carried out anneal, can improve the performance of film.Nitrogenous silicic acid magnesium film to making under the above-mentioned specific process conditions carries out anneal, and anneal comprises the process that nitrogenous silicic acid magnesium film is warming up to annealing temperature and insulation.Annealing temperature is 500 ℃～800 ℃.Anneal environment can be for rare gas element gas, like nitrogen, and argon gas etc., perhaps vacuum annealing.In a preferred embodiment of the invention, anneal is in the vacuum oven of 0.01Pa, to anneal.Annealing temperature is preferably 550 ℃～650 ℃.Annealing heats up and to be difficult for too fastly or slow excessively, and temperature rise rate is 1 ℃/min～10 ℃/min, and preferably, temperature rise rate is 5 ℃/min～8 ℃/min.After being warming up to annealing temperature, keep 1h～3h, preferably, keep 2h.Annealing has improved the crystalline quality of film, improves the luminous efficiency of film.
The embodiment of the invention also provides the application of above-mentioned nitrogenous silicic acid magnesium film in feds, cathode tube and/or electroluminescent device.With the electroluminescent device is example, sees also Fig. 2, and the organic electroluminescence device that adopts nitrogenous silicic acid magnesium film material in the foregoing description is shown, and it comprises glass-base 21, anode 22, luminescent layer 23 and the negative electrode 24 that is cascading.Anode 22 can adopt tin indium oxide (abbreviating ITO as), and luminescent layer 23 comprises the nitrogenous silicic acid magnesium film in the embodiment of the invention; Negative electrode 24 can be but be not limited to metal A g.Thereby in a specific embodiment, the membrane electro luminescent device structural table is shown: the nitrogenous silicic acid magnesium film/Ag of glass/ITO/.Each layer can adopt existing method to form, and as adopting the glass substrate that has the ITO layer, adopts the above-mentioned nitrogenous silicic acid magnesium film of magnetically controlled sputter method sputter, again vapor deposition Ag layer.
The embodiment of the invention provides a kind of nitrogenous silicic acid magnesium film, and through regulating the composition of each composition, it is high to obtain luminous intensity, the nitrogenous silicic acid magnesium film that percent crystallinity is high.The preparation method of this nitrogenous silicic acid magnesium film adopts magnetron sputtering method, has realized that thin-film light emitting intensity is high, and stable performance keeps work-ing life preferably simultaneously.And the mixed gas that adopts rare gas element and hydrogen carries out anneal to the gallium-doped zinc oxide film of sputter gained, can improve the luminous efficiency of film, more a spot of titanium doped film that just can the obtained performance excellence.
Below in conjunction with specific embodiment concrete realization of the present invention is described in detail, for making things convenient for practical application, the parameter of each powder will be described with mass percent:
Embodiment 1:
Selecting purity for use is 99.99% 7.36g MgO powder, 6g SiO
2Powder, 14g Si
3N
4Powder and 1.28g TiO
2Powder, after it was mixed, 1200 ℃ of high temperature sinterings became the ceramic target of Φ 50 * 2mm, and target is packed in the vacuum cavity.Then, successively use the glass substrate of acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning band ITO, and it is carried out oxygen plasma treatment, put into vacuum cavity.Is the distance setting of target and substrate 70mm.Be extracted into 7.0 * 10 to the vacuum tightness of cavity with mechanical pump and molecular pump
-4Pa is to the argon gas of vacuum cavity feeding and the mixed gas of hydrogen, wherein; Hydrogen content is 5% (volume ratio), and gas flow is 20sccm, and pressure is adjusted to 1.0Pa; Underlayer temperature is set at 500 ℃, and sputtering power is adjusted to 100W, and sputter obtains nitrogenous silicic acid magnesium film.The nitrogenous silicic acid magnesium film of gained is annealed in the vacuum oven of 0.01Pa, wherein, annealing temperature is 600 ℃ again, and temperature rise rate is 6 ℃/min, and soaking time is 2h.Obtain nitrogenous silicic acid magnesium film, its molecular formula is: Mg
0.92Si
2O
2N
2:
0.08Ti
4+
Embodiment 2:
Selecting purity for use is 99.99% 6.8g MgO powder, 6g SiO
2Powder, 14g Si
3N
4Powder and 2.4g TiO
2Powder, after it was mixed, 900 ℃ of high temperature sinterings became the ceramic target of Φ 50 * 2mm, and target is packed in the vacuum cavity.Then, successively use acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up, put into vacuum cavity with high pure nitrogen.Is the distance setting of target and substrate 50mm.Be extracted into 1.0 * 10 to the vacuum tightness of cavity with mechanical pump and molecular pump
-3Pa is to the argon gas of vacuum cavity feeding and the mixed gas of hydrogen, wherein; Hydrogen content is 1% (volume ratio), and gas flow is 20sccm, and pressure is adjusted to 0.2Pa; Underlayer temperature is set at 350 ℃, and sputtering power is adjusted to 100W, and sputter obtains nitrogenous silicic acid magnesium film.The nitrogenous silicic acid magnesium film of gained is annealed in the vacuum oven of 0.01Pa, wherein, annealing temperature is 500 ℃ again, and temperature rise rate is 5 ℃/min, and soaking time is 1h.Obtain nitrogenous silicic acid magnesium film, its molecular formula is: Mg
0.85Si
2O
2N
2:
0.15Ti
4+
Embodiment 3:
Selecting purity for use is 99.99% 7.92g MgO powder, 6g SiO
2Powder, 14g Si
3N
4Powder and 0.16g TiO
2Powder, after it was mixed, 1000 ℃ of high temperature sinterings became the ceramic target of Φ 50 * 2mm, and target is packed in the vacuum cavity.Then, successively use the glass substrate of acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning band ITO, and it is carried out oxygen plasma treatment, put into vacuum cavity.Is the distance setting of target and substrate 60mm.Be extracted into 6.0 * 10 to the vacuum tightness of cavity with mechanical pump and molecular pump
-4Pa is to the argon gas of vacuum cavity feeding and the mixed gas of hydrogen, wherein; Hydrogen content is 2% (volume ratio), and gas flow is 23sccm, and pressure is adjusted to 0.5Pa; Underlayer temperature is set at 400 ℃, and sputtering power is adjusted to 100W, and sputter obtains nitrogenous silicic acid magnesium film.The nitrogenous silicic acid magnesium film of gained is annealed in the vacuum oven of 0.01Pa, wherein, annealing temperature is 600 ℃ again, and temperature rise rate is 5 ℃/min, and soaking time is 1.5h.Obtain nitrogenous silicic acid magnesium film, its molecular formula is: Mg
0.99Si
2O
2N
2:
0.01Ti
4+
Embodiment 4:
Selecting purity for use is 99.99% 7.84g MgO powder, 6g SiO
2Powder, 14g Si
3N
4Powder and 0.32g TiO
2Powder, after it was mixed, 1100 ℃ of high temperature sinterings became the ceramic target of Φ 50 * 2mm, and target is packed in the vacuum cavity.Then, successively use the glass substrate of acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning band ITO, and it is carried out oxygen plasma treatment, put into vacuum cavity.Is the distance setting of target and substrate 70mm.Be extracted into 8.0 * 10 to the vacuum tightness of cavity with mechanical pump and molecular pump
-4Pa is to the argon gas of vacuum cavity feeding and the mixed gas of hydrogen, wherein; Hydrogen content is 15% (volume ratio), and gas flow is 30sccm, and pressure is adjusted to 1.0Pa; Underlayer temperature is set at 520 ℃, and sputtering power is adjusted to 30W, and sputter obtains nitrogenous silicic acid magnesium film.The nitrogenous silicic acid magnesium film of gained is annealed in the vacuum oven of 0.01Pa, wherein, annealing temperature is 650 ℃ again, and temperature rise rate is 1 ℃/min, and soaking time is 2h.Obtain nitrogenous silicic acid magnesium film, its molecular formula is: Mg
0.98Si
2O
2N
2:
0.02Ti
4+
Embodiment 5:
Selecting purity for use is 99.99% 7.64g MgO powder, 6g SiO
2Powder, 14g Si
3N
4Powder and 0.72g TiO
2Powder, after it was mixed, 1200 ℃ of high temperature sinterings became the ceramic target of Φ 50 * 2mm, and target is packed in the vacuum cavity.Then, successively use the glass substrate of acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning band ITO, and it is carried out oxygen plasma treatment, put into vacuum cavity.Is the distance setting of target and substrate 70mm.Be extracted into 6.0 * 10 to the vacuum tightness of cavity with mechanical pump and molecular pump
-4Pa is to the argon gas of vacuum cavity feeding and the mixed gas of hydrogen, wherein; Hydrogen content is 3.5% (volume ratio), and gas flow is 23sccm, and pressure is adjusted to 0.5Pa; Underlayer temperature is set at 500 ℃, and sputtering power is adjusted to 150W, and sputter obtains nitrogenous silicic acid magnesium film.Again with the nitrogenous silicic acid magnesium film of gained at AN, wherein, annealing temperature is 600 ℃, temperature rise rate is 1 ℃/min, soaking time is 2h.Obtain nitrogenous silicic acid magnesium film, its molecular formula is: Mg
0.955Si
2O
2N
2:
0.045Ti
4+
Embodiment 6:
Selecting purity for use is 99.99% 7.48g MgO powder, 6g SiO
2Powder, 14g Si
3N
4Powder and 1.04g TiO
2Powder, after it was mixed, 1300 ℃ of high temperature sinterings became the ceramic target of Φ 50 * 2mm, and target is packed in the vacuum cavity.Then, successively use the glass substrate of acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning band ITO, and it is carried out oxygen plasma treatment, put into vacuum cavity.Is the distance setting of target and substrate 90mm.Be extracted into 1.0 * 10 to the vacuum tightness of cavity with mechanical pump and molecular pump
-5Pa is to the argon gas of vacuum cavity feeding and the mixed gas of hydrogen, wherein; Hydrogen content is 15% (volume ratio), and gas flow is 30sccm, and pressure is adjusted to 4.5Pa; Underlayer temperature is set at 550 ℃, and sputtering power is adjusted to 100W, and sputter obtains nitrogenous silicic acid magnesium film.The nitrogenous silicic acid magnesium film of gained is annealed in the vacuum oven of 0.01Pa, wherein, annealing temperature is 800 ℃ again, and temperature rise rate is 10 ℃/min, and soaking time is 3h.Obtain nitrogenous silicic acid magnesium film, its molecular formula is: Mg
0.935Si
2O
2N
2:
0.065Ti
4+
Embodiment 7:
Selecting purity for use is 99.99% 7.2g MgO powder, 6g SiO
2Powder, 14g Si
3N
4Powder and 1.6g TiO
2Powder, after it was mixed, 1300 ℃ of high temperature sinterings became the ceramic target of Φ 50 * 2mm, and target is packed in the vacuum cavity.Then, successively use the glass substrate of acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning band ITO, and it is carried out oxygen plasma treatment, put into vacuum cavity.Is the distance setting of target and substrate 90mm.Be extracted into 1.0 * 10 to the vacuum tightness of cavity with mechanical pump and molecular pump
-5Pa is to the argon gas of vacuum cavity feeding and the mixed gas of hydrogen, wherein; Hydrogen content is 8% (volume ratio), and gas flow is 15sccm, and pressure is adjusted to 0.2Pa; Underlayer temperature is set at 550 ℃, and sputtering power is adjusted to 120W, and sputter obtains nitrogenous silicic acid magnesium film.The nitrogenous silicic acid magnesium film of gained is annealed in the vacuum oven of 0.01Pa, wherein, annealing temperature is 800 ℃ again, and temperature rise rate is 10 ℃/min, and soaking time is 3h.Obtain nitrogenous silicic acid magnesium film, its molecular formula is: Mg
0.9Si
2O
2N
2:
0.1Ti
4+
Fig. 3 is the electroluminescent spectrum figure of the nitrogenous silicic acid magnesium film of the embodiment of the invention 1 preparation, and it has the emission of the last one at the 500nm place.
Fig. 4 be the nitrogenous silicic acid magnesium film of the embodiment of the invention 1 preparation under 300 ℃, use the luminous intensity variations figure after 0 day, 2 days, 4 days, 6 days, 8 days, 10 days, 12 days, 14 days.As can be seen from the figure film uses a week under 300 ℃ of high temperature, still keeps original 90% luminous intensity.
Fig. 5 is the X-ray diffractogram of the nitrogenous silicic acid magnesium film of the embodiment of the invention 1 preparation.Reference standard PDF card among the figure, corresponding diffraction peak is a nitrogen-oxygen-silicon magnesium crystallization phases, the relevant peak crystallization of titanium do not occur, explains that titanium is the lattice that has got into matrix.Can find out that it is in the crystal of matrix that titanium ion is doped to the nitrogen Magnesium Silicate q-agent, does not destroy crystalline structure
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a nitrogenous silicic acid magnesium film is characterized in that, said film is titanium doped nitrogenous silicic acid magnesium film, and the chemical general formula of said titanium doped nitrogenous silicic acid magnesium film is Mg
1-XSi
2O
2N
2:
XTi
4+, wherein, the span of X is 0.01～0.15.
2. nitrogenous silicic acid magnesium film as claimed in claim 1 is characterized in that the span of said X is 0.02～0.08.
3. the preparation method of a nitrogenous silicic acid magnesium film is characterized in that, said method comprises the steps:
With MgO powder, SiO
2Powder, Si
3N
4Powder and TiO
2Powder is according to mol ratio (1-X): 0.5: 0.5: X mixes, and sintering is as target, and wherein, the span of said X is 0.01～0.15;
Said target is packed in the magnetron sputtering cavity; Vacuumize, it is 0.2Pa～4.5Pa that operating pressure is set, and feeds the mixed gas of rare gas element and hydrogen; Mixed gas flow is 15sccm～30sccm; Underlayer temperature is 350 ℃～750 ℃, and sputtering power is 30W～150W, and sputter gets nitrogenous silicic acid magnesium film.
4. the preparation method of nitrogenous silicic acid magnesium film as claimed in claim 3 is characterized in that, the span of said X is 0.02～0.08.
5. the preparation method of nitrogenous silicic acid magnesium film as claimed in claim 3 is characterized in that, the nitrogenous silicic acid magnesium film that makes is further carried out anneal.
6. the preparation method of nitrogenous silicic acid magnesium film as claimed in claim 5 is characterized in that, the annealing temperature of said anneal is 500 ℃～800 ℃, and said annealed soaking time is 1h～3h.
7. the preparation method of nitrogenous silicic acid magnesium film as claimed in claim 3 is characterized in that, the volumn concentration of hydrogen is 1%～15% in the said mixed gas.
8. the preparation method of nitrogenous silicic acid magnesium film as claimed in claim 3 is characterized in that, the volumn concentration of hydrogen is 3%～8% in the said mixed gas.
9. select the preparation method of a described nitrogenous silicic acid magnesium film like claim 3 to 8, it is characterized in that, the operating pressure of said cavity is 0.8Pa～2.5Pa, and said underlayer temperature is 400 ℃～600 ℃, and said sputtering power is 80W～120W.
10. according to claim 1 or claim 2 the application of nitrogenous silicic acid magnesium film in feds, cathode tube and/or electroluminescent device.
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| CN104178146A (en) * | 2013-05-23 | 2014-12-03 | 海洋王照明科技股份有限公司 | Manganese titanium co-doped nitrogen germanate light-emitting film and preparation method thereof and electroluminescent device |
| CN104178136A (en) * | 2013-05-23 | 2014-12-03 | 海洋王照明科技股份有限公司 | Samarium-doped nitrogen-containing silicate light-emitting film and preparation method thereof and electroluminescent device |
| CN104178145A (en) * | 2013-05-23 | 2014-12-03 | 海洋王照明科技股份有限公司 | Cerium terbium co-doped nitrogen germanate light-emitting film and preparation method thereof and electroluminescent device |
| CN104232087A (en) * | 2014-08-11 | 2014-12-24 | 北京大学工学院包头研究院 | Fluorescent material and preparation method and application thereof |
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