CN101175347A - Production method for oxide luminescent layer in inorganic electroluminescence display device - Google Patents
Production method for oxide luminescent layer in inorganic electroluminescence display device Download PDFInfo
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- CN101175347A CN101175347A CNA2007101711138A CN200710171113A CN101175347A CN 101175347 A CN101175347 A CN 101175347A CN A2007101711138 A CNA2007101711138 A CN A2007101711138A CN 200710171113 A CN200710171113 A CN 200710171113A CN 101175347 A CN101175347 A CN 101175347A
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Abstract
The present invention discloses the production method of the oxide luminous layer in a non-organic electroluminescent display, which belongs to the manufacturing technical field of the non-organic electroluminescent display driven by alternating current. The method of the present invention is that the corresponding oxide powder is directly sprayed and coated on a metal backboard to make a ceramic target. The ceramic target is sputtered on a plating film to form an oxide luminous layer film, which is applied to the non-organic electroluminescent display. With the present invention, the production cost of a large-size target used for sputtering and aggrading a large-area oxide luminous film; the crack in the ceramic target production agglutinating process is avoided; the probability of the crack in the target using process is reduced; the target component is much easier to be adjusted; and the research and development and the production costs of the display are reduced.
Description
Technical field:
The invention belongs to technical field of flat panel display, particularly a kind of inorganic EL display, the manufacture method of oxide luminescent layer in particularly a kind of inorganic EL display.
Background technology:
Characteristics such as that inorganic EL (EL) flat-panel monitor has is all solid state, in light weight, thin thickness, visual angle are big, simple in structure can be used in adverse circumstances such as low temperature, vibrations, and very wide application prospect is arranged.Inorganic EL display generally uses sulfide or oxide as luminescent layer, wherein with oxide as luminescent layer, have that the rete manufacture craft is simple, device moisture resistance gas ability strong, rich color, be easy to advantage such as large-scale production.In order to obtain meeting the practical luminous efficiency that requires, the oxide that uses the multicomponent composition usually is as luminescent layer.Vacuum magnetic control pulse sputter is to make the most frequently used, the most ripe film build method of oxide luminescent layer film at present.With ceramic target sputter in vacuum chamber of corresponding composition, film forming on glass substrate.For small-size display, can use undersized target, but film forming is even on large-sized glass substrate, efficient is high in the making of large-sized monitor requirement, this just needs the corresponding size that improves the sputter ceramic target.The manufacture method commonly used of at present traditional multi-component oxide ceramic target is: earlier with after the various compositions mixed as required, compress with isostatic cool pressing, high temperature sintering becomes tabular target again; What perhaps cost was higher directly becomes target with HIP sintering.Because large-sized ceramic target is easy to because thermal stress is cracked, so the tabular target size of sintering can not be too big in the sintering process.In order to satisfy the making requirement of large-sized monitor, a plurality of small size ceramic targets can only be spliced into a large-size target.Simultaneously, cracked in sintering process in order to prevent tabular target, also need certain thickness, can not do too thinly.In addition; in order better target to be fixed on the base (especially when target in the vertical position sputter time),, also need usually target is bundled on the metal backing during sputter coating simultaneously in order to improve cooling effect; ripe at present binding method is with the indium metal binding, but indium costs an arm and a leg.
The weak point of traditional used target manufacture method of large size electro electroluminescent display oxide luminescent layer sputter is: cost height in the ceramic target sintering process, and the cycle is long, and cracked easily in the sintering process; Large-size target needs a plurality of target splicings, further raises the cost; If the tabular pottery thickness that sintering is made is too thin, be easy to crackedly in the sintering process, if but too thick, target is cracked easily because of cooling difficulty in high power sputter use; When the ceramic target that sinters is fixed on the target base,, be difficult to guarantee that contact is good fully owing to be hard contact, this can have a strong impact on the heat radiation that the sputter use hits, make target cracked easily, and if bind with indium metal in order to improve cooling effect, then cost is higher; To the target of vertical use, for the fixed position, more need several undersized targets to be bundled on the metal backing with indium metal, cost is higher; When the composition in the target need be adjusted, need to make new target, but because new target cost of manufacture height, the cycle is long, so the composition adjustment is relatively more difficult.
Summary of the invention:
The object of the present invention is to provide the manufacture method of oxide luminescent layer in a kind of inorganic EL display, described this method will solve cost height in the ceramic target sintering process in the manufacture method of oxide luminescent layer in the inorganic EL display of the prior art, the cycle is long and sintering process in cracked technical problem easily, to solve large-size target simultaneously and need a plurality of target splicings, the technical problem that cost is high, also to solve new target cost of manufacture height, cycle is long, the difficult technical problem of adjusting of composition.
The invention provides the manufacture method of oxide luminescent layer in a kind of inorganic EL display, comprise the steps, the step that the oxide powder that will make oxide luminescent layer and need mixes according to needed proportioning; One sprays to the powder that mixes on the metal backing with plasma spraying method, makes the step of spraying target; One with spraying target magnetron sputtering in vacuum chamber, the step of deposition making oxide luminescent layer film; Oxide luminescent layer film is in air or the step of annealing in the vacuum.
Further, if making is the green glow inorganic electroluminescence device, described powder is the mixture of zinc silicate, zinc oxide, germanium oxide and manganese oxide.
Further, if making is the ruddiness inorganic electroluminescence device, described powder is the mixture of indium oxide, gallium oxide and europium oxide.
Further, with powder evenly after, sintering in advance in high temperature so that various composition reacts, it is more stable to make it to become, thereby effectively control spraying target composition departs from the starting powder composition.
Further, for the mixed-powder heating-up temperature of zinc silicate, zinc oxide, germanium oxide, manganese oxide between 1000 ℃ ~ 1500 ℃.
Further, the powder that mixes with argon ion spraying is to metal backing, and backboard is metallic copper or stainless steel.
Further, the THICKNESS CONTROL that powder is sprayed to the sprayed coating that forms on the metal backing between 0.1 ~ 10 millimeter, the too thin useful life that then influences target, the too thick cooling effect that then influences in the sputter use.
Further, powder is sprayed to the THICKNESS CONTROL of the sprayed coating that forms on the metal backing at 0.5 ~ 3 millimeter.
Further, the thickness of described oxide luminescent layer is between 100 nanometers ~ 1000 nanometers.
Further, the thickness of described oxide luminescent layer is between 300 ~ 600 nanometers.
Further, use the radio frequency magnetron sputtering method film forming.
Further, the atmosphere of carrying out magnetron sputtering in vacuum chamber is the mist of argon gas, oxygen or argon gas and oxygen.
Further, when annealing in the vacuum, aerating oxygen is to avoid the disappearance of oxygen in luminescent layer, the dielectric layer.
The invention has the advantages that: 1) for large-sized ceramic target, do not need a plurality of small size targets to be spliced to form, but can on large-sized metal backing, directly spray, the disposable target of making, save the process of powder pressure forming-high temperature sintering in the common ceramic target making like this, also avoid the frangible problem of target in the sintering process, saved the time and materials cost greatly.2) because the large scale metal backing is easy to make, and the size of spraying target can be far longer than the ceramic target that sintering forms, so the spraying target has very big advantage on size range.3) target of making of spraying process is very tight with combining of metal backing, has improved the cooling effect of target in the sputter use, simultaneously owing to being easy to control the thickness of target, so reduced the cracked probability of target in the sputter use.4), no longer need further to have reduced cost with expensive indium binding to the target of vertical use.5) if composition needs to adjust in the use, because it is low to make new spraying target cost, the cycle is short, and metal backing can also reuse, so it is much relatively easy to adjust the composition of target.
The present invention and has compared with prior art reduced the cost of manufacture of large scale oxide target material significantly, has avoided ceramic target to make cracking in the sintering process, has shortened fabrication cycle; Reduced cracked probability in the target use; The composition adjustment of target is easier, has reduced display research and development and production cost.
Description of drawings:
Fig. 1 is with the XRD diffraction pattern after the EL luminescent layer annealing of spraying target as sputter in the embodiment of the invention 1.
Fig. 2 is that 30 microseconds and frequency are the brightness-voltage curve that records under 200 hertz the ac pulse voltage for the green glow El element in the embodiment of the invention 1 in pulse duration.
Fig. 3 is the electroluminescent spectrum figure of green glow El element under the 240V ac pulse voltage in the embodiment of the invention 1.
Fig. 4 is that 30 microseconds, frequency are the brightness-voltage curve that records under 200 hertz the ac pulse voltage for the green glow El element in the embodiment of the invention 2 in pulse duration.
Fig. 5 is the electroluminescent spectrum figure of green glow El element under the 220V ac pulse voltage in the embodiment of the invention 2.
Fig. 6 is that 30 microseconds, frequency are the brightness-voltage curve that records under 200 hertz the ac pulse voltage for the green glow El element in the embodiment of the invention 3 in pulse duration.
Fig. 7 is the electroluminescent spectrum figure of green glow El element under the 200V ac pulse voltage in the embodiment of the invention 3.
Embodiment:
Below in conjunction with description of drawings embodiments of the invention are described in further detail, but present embodiment is not limited to the present invention, every employing similarity method of the present invention and similar variation thereof all should be listed protection scope of the present invention in.
The invention provides a kind of ceramic target sputter of making of spraying process and make oxide EL luminescent layer film, and apply it to method in the inorganic electroluminescent flat-panel display, reduced the cost of manufacture of large scale oxide target material significantly, reduced the probability that ftractures in the target use, the target composition is adjusted easily, reduced the cost in display device research and development and the production process.Specific embodiment is as follows:
With manganese-doped willemite (green light fluorescent powder), zinc oxide (purity 99.99%), germanium oxide (purity 99.999%), manganese oxide (purity 99.99%) powder according to 1: 1.92: 1: 0.08 mixed in molar ratio is even, spray on the oxygen-free copper backboard with argon plasma, having sprayed back green glow ceramic target thickness is 1 millimeter.
Dielectric layer barium strontium titanate under sputtering sedimentation on the transparent bottom electrode ITO on the TFT-LCD glass substrate, thickness are 300 sodium rice.The spraying target made from said method is descending sputter 400 sodium rice green glow EL luminescent layers on the dielectric layer barium strontium titanate then.The luminescent layer sputtering condition is: base vacuum is 2.7 * 10
-3Pa, Ar/O
2Than being 9: 1, sputtering pressure is 0.1Pa, and 200 ℃ of substrate temperatures, target-substrate distance are 5cm, and sputtering power density is 8.8W/cm
2The 730 ℃ of annealing one hour in vacuum annealing furnace of the intact back of sputter, aerating oxygen is to 1.2*10 in the annealing process
-2Pa.Luminescent layer moved back behind the fire the XRD test result as shown in Figure 1, part diffraction maximum wherein is from substrate, part is from the acid of the SiGe in green luminescence layer zinc composition.The XPS constituent analysis result of luminescent layer shows that the composition of green glow film is Zn
4.08Si
5.14Ge
1.82O
35.65: Mn
0.34, wherein Zn and Ge disappearance is many, and this causes in spraying system target and thin film sputtering process.Dielectric layer barium strontium titanate and tantalum pentoxide in sputter on the luminescent layer then, barium strontium titanate thickness is 400 sodium rice, tantalum pentoxide thickness is 400 sodium rice.Last deposited by electron beam evaporation 150 sodium rice aluminium top electrodes.What Fig. 2 showed is the brightness-voltage curve of this green device, and the pulse voltage pulse duration of test is 30 microseconds, and frequency is 200 hertz.That Fig. 3 shows is the electroluminescent spectrum figure of this green glow El element when applying the 240V ac pulse voltage, the spectrum coordinate is (x=0.490, y=0.501), the green light peak of spectrogram demonstration except about 540nm, also has apparent in view ruddiness peak at 608nm, wherein green light peak is from the SiGe acid zinc composition of crystallization, and the ruddiness peak is from amorphous zinc silicate composition, and this is because the disappearance of Zn and Ge causes luminescent layer partially crystallizable difficulty to cause.
Spraying target preparation method is identical with embodiment 1, but before spraying the green glow powder even after 1200 ℃ of sintering 4 hours in advance in air in advance, this is for wherein each component reacted, it is more uniform and stable to make it to become.The structure of the green glow El element of making is identical with embodiment 1.Light emitting layer thickness is 400 sodium rice, sputtering condition: base vacuum is 2.7 * 10
-3Pa, Ar/O
2Than being 9: 1, sputtering pressure is 2Pa, and 200 ℃ of substrate temperatures, target-substrate distance are 5cm, and sputtering power density is 8.8W/cm
2Implement annealing behind the sputter coating, annealing conditions is identical with embodiment 1.What Fig. 4 showed is the brightness-voltage curve of this green glow El element, and test condition is identical with embodiment 1, Fig. 5 demonstration be the electroluminescent spectrum figure of this green glow El element when applying the 220V ac pulse voltage, the spectrum coordinate be (x=0.305, y=0.647).
Spraying target preparation method is identical with embodiment 2, and the structure of the green device of making is identical with embodiment 2 with the sputtering condition of luminescent layer.Luminescent layer in vacuum annealing furnace 700 ℃ annealing one hour, aerating oxygen is to 1.2*10 in the annealing process
-2Pa.What Fig. 6 showed is the brightness-voltage curve of this green glow El element, and test condition is identical with embodiment 1, and what Fig. 7 showed is the spectrogram of this green glow El element when applying the 200V ac pulse voltage, accordingly chromaticity coordinates be (x=0.428, y=0.550).
Claims (13)
1. the manufacture method of oxide luminescent layer in the inorganic EL display is characterized in that, comprises the steps the step that the oxide powder that will make oxide luminescent layer and need mixes according to needed proportioning; One sprays to the powder that mixes on the metal backing with plasma spraying method, makes the step of spraying target; One with spraying target magnetron sputtering in vacuum chamber, the step of deposition making oxide luminescent layer film; Oxide luminescent layer film is in air or the step of annealing in the vacuum.
2. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 1, and described powder is the mixture of zinc silicate, zinc oxide, germanium oxide and manganese oxide.
3. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 1, and described powder is the mixture of indium oxide, gallium oxide and europium oxide.
4. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 1, with powder evenly after, sintering in advance in high temperature reacts various compositions.
5. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 1, for the mixed-powder heating-up temperature of zinc silicate, zinc oxide, germanium oxide, manganese oxide between 1000 ℃ ~ 1500 ℃.
6. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 1, and the powder that mixes with argon ion spraying is to metal backing, and backboard is metallic copper or stainless steel.
7. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 1, and the THICKNESS CONTROL that powder is sprayed to the sprayed coating that forms on the metal backing is between 0.1 ~ 10 millimeter.
8. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 7, and the THICKNESS CONTROL that powder is sprayed to the sprayed coating that forms on the metal backing is at 0.5 ~ 3 millimeter.
9. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 1, and the thickness of described oxide luminescent layer is between 100 nanometers ~ 1000 nanometers.
10. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 9, and the thickness of described oxide luminescent layer is between 300 ~ 600 nanometers.
11. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 1, uses the radio frequency magnetron sputtering method film forming.
12. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 11, the atmosphere of carrying out magnetron sputtering in vacuum chamber is the mist of argon gas, oxygen or argon gas and oxygen.
13. the manufacture method of oxide luminescent layer is characterized in that in a kind of inorganic EL display according to claim 1, when annealing in a vacuum, and aerating oxygen.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102796517A (en) * | 2011-05-23 | 2012-11-28 | 海洋王照明科技股份有限公司 | Nitrogenous magnesium silicate film, and preparation method and application thereof |
| CN103993281A (en) * | 2014-05-30 | 2014-08-20 | 天津大学 | Preparation method of FTO (F-doped SiO2) transparent conducting thin film |
| CN104152853A (en) * | 2014-07-08 | 2014-11-19 | 中国人民解放军国防科学技术大学 | Glass ceramic target material and preparation method thereof |
-
2007
- 2007-11-28 CN CNA2007101711138A patent/CN101175347A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102796517A (en) * | 2011-05-23 | 2012-11-28 | 海洋王照明科技股份有限公司 | Nitrogenous magnesium silicate film, and preparation method and application thereof |
| CN102796517B (en) * | 2011-05-23 | 2015-02-04 | 海洋王照明科技股份有限公司 | Nitrogenous magnesium silicate film, and preparation method and application thereof |
| CN103993281A (en) * | 2014-05-30 | 2014-08-20 | 天津大学 | Preparation method of FTO (F-doped SiO2) transparent conducting thin film |
| CN104152853A (en) * | 2014-07-08 | 2014-11-19 | 中国人民解放军国防科学技术大学 | Glass ceramic target material and preparation method thereof |
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Application publication date: 20080507 |