CN103137885A - Composite packaging structure and packaging method for organic light-emitting devices - Google Patents
Composite packaging structure and packaging method for organic light-emitting devices Download PDFInfo
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- CN103137885A CN103137885A CN2011103824993A CN201110382499A CN103137885A CN 103137885 A CN103137885 A CN 103137885A CN 2011103824993 A CN2011103824993 A CN 2011103824993A CN 201110382499 A CN201110382499 A CN 201110382499A CN 103137885 A CN103137885 A CN 103137885A
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Abstract
The invention provides a composite packaging structure and a packaging method for organic light-emitting devices. The composite packaging structure comprises an anode substrate, a functional layer, a luminous layer, a metal cathode and a packaging layer, wherein the anode substrate and the packaging layer form a closed space; the functional layer, the luminous layer and the metal cathode are accommodated in the closed space; the packaging layer sequentially comprises a nitride membrane, an oxide membrane and a PET membrane loaded with metallic aluminum; the oxide membrane is formed by mixing one or more of a SiO2 membrane, a GeO2 membrane and a SnO2 membrane with one or more of metallic elements of Ca, Ba, Sr and Mg; and a SiO membrane serving as a protective layer is arranged between the metal cathode and the nitride membrane. The composite packaging structure can effectively reduce the corrosion of moisture to the organic light-emitting devices, obviously prolong the service life of the organic light-emitting devices, and can protect the metal cathode from damage. The packaging method is particularly used for packaging flexible organic light-emitting devices.
Description
Technical field
The invention belongs to organic electroluminescence device, be specifically related to a kind of compound encapsulation structure and method for packing thereof of organic electroluminescence device.
Background technology
Organic electroluminescence device (OLED) is based on a kind of current mode light emitting semiconductor device of organic material.Its typical structure is to accompany multilayer organic material film (hole injection layer, hole transmission layer, luminescent layer, electron supplying layer and electron injecting layer) between transparent anode and metallic cathode, and after applying certain voltage between electrode, luminescent layer will be luminous.In recent years, the characteristics such as organic electroluminescence device is low due to cost of manufacture own, the response time is short, luminosity is high, wide visual angle, low driving voltage and energy-conserving and environment-protective have been subject to extensive concern in fields such as panchromatic demonstration, backlight and illuminations, and are considered to be most likely at the device of new generation that occupies the dominance on following illumination and display device market.
At present, the problem that the organic electroluminescence device average life is shorter, this is mainly because organic material film is very loose, occurs rapidly aging after easily being infiltrated by compositions such as airborne steam and oxygen.Therefore, organic electroluminescence device must encapsulate before entering actual use, and the quality of encapsulation is directly connected to the life-span of organic electroluminescence device.
Adopt glass cover or crown cap to encapsulate in conventional art, its edge is resin-sealed with ultraviolet polymerization, but the glass cover that uses in this method or crown cap volume are often larger, have increased the weight of device, and the method can not be applied to the give out light encapsulation of device of flexible organic electroluminescence.At present, have been reported introduction with SiN
XOr SiO
XBe arranged on the metallic cathode surface etc. inorganic material by methods such as magnetron sputterings, as the encapsulated layer of organic electroluminescence device, but under the high-temperature operation condition of magnetron sputtering, the metallic cathode surface is subject to destruction.
Summary of the invention
For overcoming the defective of above-mentioned prior art, the invention provides a kind of compound encapsulation structure and method for packing thereof of organic electroluminescence device.This compound encapsulation structure can reduce steam effectively to the erosion of organic electroluminescence device, improves significantly the life-span of organic electroluminescence device, and can protect metallic cathode to exempt from destruction.The inventive method is applicable to encapsulate the organic electroluminescence device with the conducting glass substrate preparation, also is applicable to the flexible organic electroluminescent device of encapsulation take plastics (for example PET film) or metal as the substrate preparation.The inventive method is particularly useful for encapsulating flexible organic electroluminescent device.
On the one hand, the invention provides a kind of compound encapsulation structure of organic electroluminescence device, comprise anode substrate, functional layer, luminescent layer, metallic cathode and encapsulated layer, anode substrate and encapsulated layer form an enclosure space, functional layer, luminescent layer and metallic cathode are contained in this enclosure space, wherein, described encapsulated layer comprises that successively nitride film, oxidation film and load have the high temperature resistance polyester film of metallic aluminium, and oxidation film is SiO
2, GeO
2And SnO
2One or more in film and doped with the film of one or more formation in metallic element Ca, Ba, Sr and Mg are provided with the SiO film as protective layer between metallic cathode and nitride film.
Preferably, anode substrate is conducting glass substrate or conducting PET film (high temperature resistance polyester film) substrate.
Functional layer generally includes hole injection layer, hole transmission layer, electron transfer layer and electron injecting layer.Luminescent layer is arranged between hole transmission layer and electron transfer layer.Preferably, functional layer and luminescent layer are by the method for vacuum evaporation or the method setting of solution coating.
Metallic cathode can be non-transparent metals negative electrode (aluminium, silver, gold etc.), also can be transparent cathode (dielectric layer/metal level/dielectric layer etc.).
Encapsulated layer comprises that successively nitride film, oxidation film and load have the high temperature resistance polyester film (PET film) of metallic aluminium.
Nitride film can extend water oxygen permeation pathway.Preferably, nitride film is SiN film, Si
3N
4Film or AlN film.Preferably, nitride film is individual layer, and the thickness of individual layer is 100～150nm.Nitride film also can be two-layer or multilayer.
Oxidation film is SiO
2, GeO
2And SnO
2One or more in film and doped with the film of one or more formation in metallic element Ca, Ba, Sr and Mg.Ca, Ba, Sr and Mg are the high-hydroscopicity material, at SiO
2, GeO
2And SnO
2One or more of adulterating in one or more in film in Ca, Ba, Sr and Mg can reduce steam effectively to the erosion of organic electroluminescence device, improve significantly the life-span of organic electroluminescence device.Preferably, oxidation film is individual layer, and the thickness of individual layer is 100～150nm.Oxidation film also can be two-layer or multilayer.One or more of adulterating in oxidation film in Ca, Ba, Sr and Mg can strengthen water and oxygen barrier property.Preferably, in oxidation film, the quality of doped metallic elements accounts for 15～30% of oxidation film gross mass.
Be provided with the SiO film as protective layer between metallic cathode and nitride film.The existence of SiO film can protect metallic cathode to exempt from destruction under the high-temperature operation condition of follow-up magnetron sputtering.Preferably, the thickness of SiO film is 100～150nm.
Preferably, UV glue is epoxy resin.Preferably, the thickness of UV glue is 1～1.5 μ m.
On the other hand, the invention provides a kind of method for packing of organic electroluminescence device, comprise the following steps:
(1) prepare functional layer, luminescent layer and metallic cathode on anode substrate;
(2) mode by vacuum evaporation at metallic cathode surface preparation SiO film as protective layer;
(3) pass through the mode of magnetron sputtering at SiO film surface preparation nitride film;
(4) mode of passing through magnetron sputtering is at nitride film surface preparation oxidation film, and oxidation film is SiO
2, GeO
2And SnO
2One or more in film and doped with the film of one or more formation in metallic element Ca, Ba, Sr and Mg;
(5) the high temperature resistance polyester film of metallic aluminium is arranged in nitride film surface preparation load;
(6) high temperature resistance polyester film and the anode substrate edge-coating UV glue of metallic aluminium are arranged in SiO film, nitride film, oxidation film, load, the dry sclerosis of mode UV glue by ultraviolet curing, then be cured with UV light, sealing forms an enclosure space, and functional layer, luminescent layer and metallic cathode are contained in this enclosure space.
Step (1) is for preparing functional layer, luminescent layer and metallic cathode on anode substrate.
Preferably, anode substrate is conducting glass substrate or conducting PET film (high temperature resistance polyester film) substrate.
Functional layer generally includes hole injection layer, hole transmission layer, electron transfer layer and electron injecting layer.Luminescent layer is arranged between hole transmission layer and electron transfer layer.Preferably, functional layer and luminescent layer are by the method for vacuum evaporation or the method setting of solution coating.
Metallic cathode can be non-transparent metals negative electrode (aluminium, silver, gold etc.), also can be transparent cathode (dielectric layer/metal level/dielectric layer etc.).
Step (2) prepares the SiO film as protective layer for the mode by vacuum evaporation on the metallic cathode surface.The existence of SiO film can protect metallic cathode to exempt from destruction under the high-temperature operation condition of follow-up magnetron sputtering.Preferably, the thickness of SiO film is 100～150nm.
Step (3) is to pass through the mode of magnetron sputtering at SiO film surface preparation nitride film.Nitride film can extend water oxygen permeation pathway.Preferably, the base vacuum degree in step (3) magnetron sputtering process is 2 * 10
-4Pa.Preferably, nitride film is SiN film, Si
3N
4Film or AlN film.Preferably, nitride film is individual layer, and the thickness of individual layer is 100～150nm.Nitride film also can be two-layer or multilayer.
Step (4) is to pass through the mode of magnetron sputtering at nitride film surface preparation oxidation film, and oxidation film is SiO
2, GeO
2And SnO
2One or more in film and doped with the film of one or more formation in metallic element Ca, Ba, Sr and Mg.Ca, Ba, Sr and Mg are the high-hydroscopicity material, at SiO
2, GeO
2And SnO
2One or more extended water oxygen permeation pathway in one or more in film in doped metallic elements Ca, Ba, Sr and Mg reduce steam effectively to the erosion of organic electroluminescence device, improve significantly the life-span of organic electroluminescence device.
Preferably, the quality of doped metallic elements accounts for 15～30% of oxidation film gross mass.
Preferably, oxidation film is individual layer, and the thickness of individual layer is 100～150nm.Oxidation film also can be two-layer or multilayer.
Preferably, step (4) is at least a target in employing Si, Ge and Sn and at least a magnetron sputtering that carries out in Ca, Ba, Sr and Mg.Preferably, pass into oxygen and argon gas in step (4) magnetron sputtering process, the oxygen volume content accounts for 1%～15% of total gas volume.More preferably, pass into the oxygen volume content in step (4) magnetron sputtering process and account for 8% of total gas volume.Preferably, the base vacuum degree in step (4) magnetron sputtering process is 2 * 10
-4Pa.
Step (5) is for there being the high temperature resistance polyester film (PET film) of metallic aluminium in nitride film surface preparation load.
Step (6) is for having high temperature resistance polyester film (PET film) and the anode substrate edge-coating UV glue of metallic aluminium in SiO film, nitride film, oxidation film, load, the dry sclerosis of mode UV glue by ultraviolet curing, then be cured with UV light, sealing forms an enclosure space, and functional layer, luminescent layer and metallic cathode are contained in this enclosure space.
Preferably, UV glue is epoxy resin.Preferably, the thickness of UV glue is 1～1.5 μ m.
Preferably, the light intensity 10～15mW/cm of UV light
2, time for exposure 300～400s.
The present invention can pass through repeatedly repeating step (3) and (4) form the multilayer encapsulation layer, thereby reaches good packaging effect.
The compound encapsulation structure and the method for packing thereof that the invention provides a kind of organic electroluminescence device have following beneficial effect:
(1) compound encapsulation structure of the present invention can reduce steam effectively to the erosion of organic electroluminescence device, improves significantly the life-span of organic electroluminescence device, and can protect metallic cathode to exempt from destruction;
(2) the inventive method is applicable to encapsulate take electro-conductive glass as anode substrate the organic electroluminescence device of preparation, also is applicable to the flexible organic electroluminescent device of encapsulation take plastics (for example PET film) or metal as the anode substrate preparation.The inventive method is particularly useful for encapsulating flexible organic electroluminescent device;
(3) compound encapsulation structure material of the present invention is cheap, and method for packing technique is simple, and easily large tracts of land preparation is suitable for large-scale industrialization and uses.
Description of drawings
Fig. 1 is the structural representation of the compound encapsulation structure of the embodiment of the present invention 1 organic electroluminescence device;
Fig. 2 is the life-span attenuation curve figure of the compound encapsulation structure of the embodiment of the present invention 6～8 organic electroluminescence devices.
Embodiment
The following stated is the preferred embodiment of the present invention.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also make some improvement and adjustment, these improvement and adjustment also are considered as in protection scope of the present invention.
Embodiment 1:
Fig. 1 is the structural representation of the compound encapsulation structure of the present embodiment organic electroluminescence device.
A kind of compound encapsulation structure of organic electroluminescence device, as shown in Figure 1, comprise successively conducting PET film (high temperature resistance polyester film) substrate 1, hole injection layer 2, hole transmission layer 3, luminescent layer 4, electron transfer layer 5, electron injecting layer 6, metallic cathode 7 and encapsulated layer 8.Conducting PET film (high temperature resistance polyester film) substrate 1 and encapsulated layer 8 form an enclosure space by epoxy sealing, and hole injection layer 2, hole transmission layer 3, luminescent layer 4, electron transfer layer 5, electron injecting layer 6 and metallic cathode 7 are contained in this enclosure space.Described encapsulated layer 8 comprises that successively a layer thickness is that the SiO film 81 of 100nm, SiN film 82 that a layer thickness is 150nm, one deck are doped with the SnO of Sr
2Film 83 is (doped with the SnO of Sr
2Film is oxidation film, and the oxidation film gross mass is 0.8g, and the quality of Sr accounts for 15% of oxidation film gross mass, and oxide film thickness is 100nm) and load the PET film 84 of metallic aluminium is arranged.The thickness of epoxy resin is 1 μ m.The water oxygen permeability of the organic electroluminescence device after the present embodiment composite package (WVTR, g/m
2Day) be 5.3E
-4
Embodiment 2:
A kind of compound encapsulation structure of organic electroluminescence device comprises conducting glass substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, metallic cathode and encapsulated layer.Conducting glass substrate and encapsulated layer form an enclosure space by epoxy sealing, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and metallic cathode are contained in this enclosure space.Described encapsulated layer comprises that successively (oxidation film is the GeO doped with Ba to the oxidation film that a layer thickness is the SiO film of 150nm, AlN film that a layer thickness is 150nm, a layer thickness is 150nm
2Film, oxidation film gross mass are 1g, the quality of Ba account for the oxidation film gross mass 30%) and load the PET film of metallic aluminium is arranged.The thickness of epoxy resin is 1 μ m.The water oxygen permeability of the organic electroluminescence device after the present embodiment composite package (WVTR, g/m
2Day) be 3E
-4
Embodiment 3:
A kind of compound encapsulation structure of organic electroluminescence device comprises conducting glass substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, metallic cathode and encapsulated layer.Conducting glass substrate and encapsulated layer form an enclosure space by epoxy sealing, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and metallic cathode are contained in this enclosure space.Described encapsulated layer comprises that successively a layer thickness is the SiO film of 150nm, three layers of Si
3N
4Film (Si
3N
4The thickness in monolayer of film is 100nm), a layer thickness is that (oxidation film is the SiO of doped with Mg for the oxidation film of 150nm
2Film, oxidation film gross mass are 1.1g, the quality of Mg account for the oxidation film gross mass 20%) and load the PET film of metallic aluminium is arranged.The thickness of epoxy resin is 1 μ m.The water oxygen permeability of the organic electroluminescence device after the present embodiment composite package (WVTR, g/m
2Day) be 4.2E
-4
Embodiment 4:
A kind of compound encapsulation structure of organic electroluminescence device comprises conducting glass substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, metallic cathode and encapsulated layer.Conducting glass substrate and encapsulated layer form an enclosure space by epoxy sealing, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and metallic cathode are contained in this enclosure space.Described encapsulated layer comprise successively a layer thickness be 150nm the SiO film, (be respectively thickness in monolayer is SiN film, the Si of 100nm to three layers of nitride film
3N
4Film and AlN film), a layer thickness be 100nm oxidation film (oxidation film for the doping Ca, Ba SiO
2Film, oxidation film gross mass are 1g, the quality of Ca, Ba account for respectively this oxidation film gross mass 17% and 13%) and load the PET film of metallic aluminium is arranged.The thickness of epoxy resin is 1.5 μ m.The water oxygen permeability of the organic electroluminescence device after the present embodiment composite package (WVTR, g/m
2Day) be 2.5E
-4
Embodiment 5:
A kind of compound encapsulation structure of organic electroluminescence device comprises conducting glass substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, metallic cathode and encapsulated layer.Conducting glass substrate and encapsulated layer form an enclosure space by epoxy sealing, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and metallic cathode are contained in this enclosure space.Described encapsulated layer comprises that successively a layer thickness is that SiO film, a layer thickness of 150nm is the Si of 150nm
3N
4Film, a layer thickness are that (oxidation film is for doped with the SiO of Ca, Ba, Sr and Mg for the oxidation film of 150nm
2Film, oxidation film gross mass are 1.2g, the quality of Ca, Ba, Sr and Mg account for respectively the oxidation film gross mass 9%, 4%, 6% and 7%) and load the PET film of metallic aluminium is arranged.The thickness of epoxy resin is 1 μ m.The water oxygen permeability of the organic electroluminescence device after the present embodiment composite package (WVTR, g/m
2Day) be 2.1E
-4
Embodiment 6:
A kind of method for packing of organic electroluminescence device comprises the following steps:
(1) prepare functional layer, luminescent layer and metallic cathode on anode substrate
A. the pre-treatment of conducting glass substrate
Get ito glass substrate, carrying out successively liquid detergent cleaning, ethanol cleaning, acetone cleaning and pure water cleans, all clean with supersonic wave cleaning machine, each washing is adopted and was cleaned 5 minutes, stops 5 minutes, repeats respectively the method for 3 times, and then stand-by with oven for drying, also need carry out surface activation process to the ito glass substrate after cleaning, to increase the oxygen content of ito glass substrate superficial layer, improve the work function on ito glass substrate surface; ITO thickness 100nm;
B. the preparation of functional layer, luminescent layer and metallic cathode
Adopt the method for vacuum evaporation or the method for solution coating to form successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer on ito glass substrate; Adopt evaporation to make the aluminium negative electrode;
(2) mode by vacuum evaporation be prepared with one deck 100nm on the metallic cathode surface the SiO film as protective layer, vacuum degree control is 5 * 10
-5Pa, evaporation rate is
(3) mode by magnetron sputtering is utilized the Si target on SiO film surface, passes into Ar and N
2,, N
2Proportion is 8%, preparation one deck Si
3N
4Film, thickness 100nm, the base vacuum degree in magnetron sputtering process is 2 * 10
-4Pa;
(4) pass through the mode of magnetron sputtering at Si
3N
4Utilize Si target and Ca target on the film surface, magnetron sputtering is made, and passes into oxygen and argon gas, and the oxygen volume content accounts for 8% of total gas volume, base vacuum degree 2 * 10
-4Pa, preparation one deck is doped with the SiO of Ca
2Film, oxidation film gross mass are 0.9g, and Ca accounts for 30% of oxidation film gross mass, thickness 100nm;
(5) at the SiO doped with Ca
2The preparation load of film surface has the PET film of metallic aluminium;
(6) at SiO film, Si
3N
4Film, doped with the SiO of Ca
2Film, load have PET film and the ito glass substrate edge-coating epoxy resin of metallic aluminium, (thickness 1 μ m), by the dry hardening epoxy resin of the mode of ultraviolet curing (UV-Curing), then with UV light (λ=365nm) be cured, light intensity 11mW/cm
2Time for exposure 300s, sealing forms an enclosure space, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and aluminium negative electrode are contained in this enclosure space, the water oxygen permeability of the organic electroluminescence device after the present embodiment composite package (WVTR, g/m
2Day) be 2.4E
-4
Embodiment 7:Ca accounts for 22% of oxidation film gross mass, and other is with embodiment 6, the water oxygen permeability of the organic electroluminescence device after the present embodiment composite package (WVTR, g/m
2Day) be 2.9E
-4
Embodiment 8:Ca accounts for 15% of oxidation film gross mass, and other is with embodiment 6, the water oxygen permeability of the organic electroluminescence device after the present embodiment composite package (WVTR, g/m
2Day) be 3.9E
-4
Embodiment 9: step (3) repeats 2 times, and step (4) repeats 2 times, and other is with embodiment 6, the water oxygen permeability of the organic electroluminescence device after the present embodiment composite package (WVTR, g/m
2Day) be 4.4E
-4
Embodiment 10: step (3) repeats 3 times, and step (4) repeats 3 times, and other is with embodiment 6, the water oxygen permeability of the organic electroluminescence device after the present embodiment composite package (WVTR, g/m
2Day) be 3.4E
-4
Effect embodiment
Be the compound encapsulation structure of valid certificates organic electroluminescence device of the present invention and the beneficial effect of method for packing thereof, provide the related experiment data as follows.
Table 1. embodiment 6～8 compound encapsulation structure life-span attenuation
Table 1 is embodiment 6～8 compound encapsulation structure life-span attenuation table.Fig. 2 is embodiment 6～8 attenuation life-span in compound encapsulation structure life-span attenuation curve figure.
Can find out from table 1 and Fig. 2, the initial brightness of the organic electroluminescence device after composite package of the present invention is 1,000cd/m
2Under, the life-span reached more than 10,000 hours.
Can find out from above-mentioned experimental data, the water oxygen permeability of the organic electroluminescence device after composite package of the present invention (WVTR) reaches 10
-4g/m
2Day.
To sum up, the compound encapsulation structure of organic electroluminescence device provided by the invention can reduce steam effectively to the erosion of organic electroluminescence device, improves significantly the life-span of organic electroluminescence device, and can protect metallic cathode to exempt from destruction.
Claims (10)
1. the compound encapsulation structure of an organic electroluminescence device, comprise anode substrate, functional layer, luminescent layer, metallic cathode and encapsulated layer, anode substrate and encapsulated layer form an enclosure space, functional layer, luminescent layer and metallic cathode are contained in this enclosure space, it is characterized in that, described encapsulated layer comprises that successively nitride film, oxidation film and load have the high temperature resistance polyester film of metallic aluminium, and oxidation film is SiO
2, GeO
2And SnO
2One or more in film and doped with the film of one or more formation in metallic element Ca, Ba, Sr and Mg are provided with the SiO film as protective layer between metallic cathode and nitride film.
2. compound encapsulation structure as claimed in claim 1, is characterized in that, described nitride film is SiN film, Si
3N
4Film or AlN film.
3. compound encapsulation structure as claimed in claim 1, is characterized in that, the thickness of described SiO film is 100～150nm.
4. compound encapsulation structure as claimed in claim 1, is characterized in that, the quality of described doped metallic elements accounts for 15～30% of oxidation film gross mass.
5. compound encapsulation structure as claimed in claim 1, is characterized in that, described oxidation film is individual layer, and the thickness of individual layer is 100～150nm.
6. the method for packing of an organic electroluminescence device, is characterized in that, comprises the following steps:
(1) prepare functional layer, luminescent layer and metallic cathode on anode substrate;
(2) mode by vacuum evaporation at metallic cathode surface preparation SiO film as protective layer;
(3) pass through the mode of magnetron sputtering at SiO film surface preparation nitride film;
(4) mode of passing through magnetron sputtering is at nitride film surface preparation oxidation film, and oxidation film is SiO
2, GeO
2And SnO
2One or more in film and doped with the film of one or more formation in metallic element Ca, Ba, Sr and Mg;
(5) the high temperature resistance polyester film of metallic aluminium is arranged in nitride film surface preparation load;
(6) high temperature resistance polyester film and the anode substrate edge-coating UV glue of metallic aluminium are arranged in SiO film, nitride film, oxidation film, load, the dry sclerosis of mode UV glue by ultraviolet curing, then be cured with UV light, sealing forms an enclosure space, and functional layer, luminescent layer and metallic cathode are contained in this enclosure space.
7. method for packing as claimed in claim 6, is characterized in that, described in step (2), the thickness of SiO film is 100～150nm.
8. method for packing as claimed in claim 6, is characterized in that, described in step (3), nitride film is SiN film, Si
3N
4Film or AlN film.
9. method for packing as claimed in claim 6, is characterized in that, described in step (4), the quality of doped metallic elements accounts for 15～30% of oxidation film gross mass.
10. method for packing as claimed in claim 6, is characterized in that, described in step (4), oxidation film is individual layer, and the thickness of individual layer is 100～150nm.
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Application publication date: 20130605 |