CN1329458A - Preparation method of organic electroluminescent device - Google Patents
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- 238000000034 method Methods 0.000 claims abstract description 25
- 239000012044 organic layer Substances 0.000 claims abstract description 22
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- 239000012528 membrane Substances 0.000 claims description 7
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 5
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Abstract
The present invention designs a preparation method of organic electroluminescent device, and is characterized by that on the first electrode pattern of the said device the invented trapezoidal insulating columns (isolating columns) with large upper end and small lower end are prepared, then the organic layer and metal layer are vapour-deposited in turn, and the shadow effect of the insualting columns can effectively partition the second electrode of the said device. This inverted trapezoidal insulating column can be prepared by means of the procedures of rotatively coating insulating polymer film twice, one exposure and developing twice. This invented method is simple in preparation process, low in cost and high in finished product ratio.
Description
The present invention relates to a kind of preparation method of organic electroluminescence device, belong to electronic semi-conductor's components and parts technical field.
Organic electroluminescence device usually like this constitutes: first electrode (transparency electrode) of printing opacity, be deposited on the organic electroluminescent medium on first electrode and be positioned at second electrode (metal electrode) above the organic electroluminescent medium.Transparency electrode is as the anode of device, and metal electrode is as the negative electrode of device.Apply high level to transparency electrode, apply low level to metal electrode and make device luminous.One group of anode parallel to each other (negative electrode) constitutes two-dimentional X-Y addressing matrix with one group of vertical with it negative electrode parallel to each other (anode).
The pattern wiring of normally transparent electrode is realized by photoetching technique.The pattern wiring of metal electrode adopts the method for metal mask evaporation or the method for photoetching to realize.But the complex manufacturing technology of metal mask plate, cost height in the pattern wiring of metal electrode, lines are difficult for running business into particular one, and realize having difficulties on the high-resolution at device.Metal mask plate contacts with organic membrane and destroys organic layer easily simultaneously, causes the short circuit of the sun of transparency electrode and metal electrode.If carry out metal line with the method for photoetching, can have following problem again: 1. the baking temperature of photoresist (120 ℃) can make organic membrane be damaged.2. the developer solution in the photoetching, corrosive liquid can damage organic membrane.3. if adopt dry etching, the organic membrane of can breaking of the particle flux in the dry etching.More than these destructive factors finally can make the device property deterioration.
Adopt the insulated column technology to carry out the pattern wiring of metal electrode among the Japan Patent 10-106747.Device architecture such as Fig. 1: deposit transparent conductive film 2 on transparency carrier 1 makes transparent conductive film 2 by lithography one group of array that is parallel to each other.On transparent conductive film 2, adopt the method for plasma chemical enhancement mode vapor deposition (PECVD) to prepare silicon nitride (SiN) 3, silicon dioxide (SiO continuously
2) 4, silicon nitride (SiN) 5.After applying photoresist on the silicon nitride 5, make by lithography one group with transparent conductive film 2 vertical element parallel to each other of quadrature mutually.Figure with silicon nitride 5 is a mask then, uses hydrofluoric acid (HF) wet etching to go out the figure of silicon dioxide 4.Last dry etching again goes out the figure of silicon nitride 3.Direct deposit organic layer and metal level on silicon nitride 3, silicon dioxide 4, silicon nitride 5 three-layer insulated films.Silicon nitride 3, silicon dioxide 4, silicon nitride 5 three-layer insulated films have the shape of similar inverted ladder type as the insulated column of device.Because shadow effect continues the evaporation organic layer on device and metal level does not form film at the side surface of insulated column, has guaranteed the electric insulation between the adjacent image point.But this scheme has following shortcoming:
(1) insulated column is made up of three layers of inoranic membrane (silicon nitride 3-silicon dioxide 4-silicon nitride 5), needs to adopt plasma enhanced chemical vapor deposition (PECVD) method deposition film.The PECVD apparatus expensive, film-forming process complexity, process conditions are wayward, cause that rate of finished products is low in large-scale production, cost is high.
(2) in the reacting furnace of PECVD equipment, need to feed silane, nitrogen and oxygen, form silicon nitride and silicon dioxide by chemical reaction.Silane is poisonous, and the reacting furnace of equipment and gas piping need perform seal operation.Gaseous emission should be noted environmental protection simultaneously.These work meetings increase production cost.
(3) the insulated column shape realizes by single exposure, wet etching silicon dioxide 4 and twice dry etching silicon nitride 3 and 5.Figure complicated process of preparation, process conditions are wayward, cause that rate of finished products is low in the large-scale production, cost is high.
The objective of the invention is to propose a kind of preparation method of organic electroluminescence device, shortcomings such as, cost height low at the complex process, the rate of finished products that exist among the insulated column preparation technology in the past provide a kind of and have passed through twice rotation and apply the simple effective method that insulating polymer film, single exposure and twice development prepare insulated column.Reach the purpose of simplifying technology, reducing cost.
The preparation method of the organic electroluminescence device that the present invention proposes may further comprise the steps:
(1) on transparent glass substrate or flexible base, board deposit transparent conductive film tin indium oxide (hereinafter to be referred as ITO) or zinc oxide (ZnO) etc. as first electrode of device, thickness is 20nm～250nm, the square resistance of conducting film is 5 Ω～70 Ω, on transparent conductive film, make one group of vertical element that is parallel to each other and separates then by lithography, making the width (being live width) of first electrode is 50 μ m～1.5mm, gap (being the lines gaps) between the electricity level is 5 μ m～120 μ m, cleans through acetone ethanol;
(2) rotation simultaneously applies first insulating barrier on the gap between above-mentioned first electrode and the electricity level, and as plain edition polyimides, Photosensitive polyimides etc., the thickness of first insulating barrier is 1 μ m～5 μ m, baking 10min～60min under 70 ℃～300 ℃;
(3) continue rotation on above-mentioned first insulating barrier and apply second insulating barrier, as Photosensitive polyimides or negative photoresist etc., the thickness of second insulating barrier is 0.5 μ m～3 μ m, toasts 10min～60min down at 70 ℃～300 ℃;
(4) above-mentioned second insulating barrier is directly carried out photoetching, form and above-mentioned transparent first electrode vertical element a plurality of parallel to each other of quadrature mutually, wherein developing time is 30s～2min, the width that makes second insulating barrier is 5 μ m～120 μ m, the gap is 50 μ m～1.5mm, toasts 10min～40min down at 70 ℃～300 ℃;
(5) figure with above-mentioned second insulating barrier is a mask, first insulating barrier develop is formed and above-mentioned transparent first electrode vertical element a plurality of parallel to each other of quadrature mutually, developing time is 30s～2min, the edge that makes first insulating barrier is than the inside 1 μ m～20 μ m of contraction in the edge of second insulating barrier, the width of first insulating barrier upper end is 3 μ m～110 μ m, the gap is 60 μ m～1.6mm, (first insulating barrier and second insulating barrier form the up big and down small trapezoidal insulated column that falls together), above-mentioned two insulating barriers are toasted, baking temperature is 70 ℃～300 ℃, and the time is 10min～60min;
(6) on above-mentioned second insulating barrier and removed evaporation organic layer on the transparent conductive film of two-layer insulating polymer and the transparent conductive film lines gap, organic layer can be made up of single or multiple lift; Single layer structure such as 8-hydroxyquinoline aluminum are (hereinafter to be referred as Alq
3), N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4,4-diamines (hereinafter to be referred as NPB) etc.; Sandwich construction is as successively by ketone peptide cyanogen (hereinafter to be referred as CuPc), NPB and Alq
3Form or successively by CuPc, NPB, Alq
3: 4-methylene dicyanoethyl-2-methyl-6-(p-dimethylamino styryl)-4H-pyrans (hereinafter to be referred as DCM) composition etc.The evaporation speed of organic membrane is 0.1nm/s～0.5nm/s, and the CuPc thickness is 5nm～30nm, and the NPB thickness is 30nm～70nm, Alq
3Thickness is 30nm～80nm, and DCM is at Alq
3In doping be 1%～10%;
(7) evaporated metal layer on above-mentioned organic layer, as be followed successively by Mg-Ag alloy and Ag, or LiF and Al etc. are as second electrode of device, Mg-Ag alloy thickness is 80nm～200nm, the Ag thickness is 20nm～100nm, and the LiF thickness is 0.2nm～1nm, and the Al thickness is 100nm～200nm.The evaporation speed of metal film is 0.1nm/s～1.5nm/s.
Dot matrix device by above prepared has following advantage:
(1) insulated column is made up of two-layer dielectric film, by the preparation of rotation painting method.Film-forming process is simple, and rate of finished products height, cost are low in large-scale production.
(2) the insulated column shape realizes by single exposure, twice development.Figure preparation technology is simple, easy control of process conditions.Rate of finished products height, cost are low in large-scale production.Be particularly useful for the preparation of high-resolution dot matrix screen.
The metal level of device prepared by this method can be separated effectively by insulated column, and device is luminous evenly, and it is low to play bright voltage.
Description of drawings:
Fig. 1 is an organic electroluminescence device section of structure in the prior art.
Fig. 2 is an organic electroluminescence device section of structure among the present invention.
Fig. 3 is an organic electroluminescence device vertical view among the present invention.
Fig. 4 a-Fig. 4 d is the preparation flow figure (part sectioned view of AA direction among Fig. 3) of isolating column of organic electroluminescent device among the present invention.
Among above-mentioned Fig. 1～Fig. 4, the 1st, transparency carrier, 2 is first electrodes, the 3rd, silicon nitride, the 4th, silicon dioxide, the 5th, silicon nitride, the 6th, organic layer, 7 second electrodes, 8 is first insulating barriers, 9 is second insulating barriers.
Elaborate content of the present invention below in conjunction with drawings and Examples.
Embodiment one:
Sputter layer of transparent conducting film ITO on transparent glass substrate, thickness is 200nm, and square resistance is 15 Ω, and photoetching forms one group of vertical element parallel to each other, and live width is that 0.22mm, lines gap are 20 μ m.Rotation applies the first insulating barrier plain edition polyimides after acetone ethanol is cleaned, and thickness is 3 μ m, rotates behind the baking 20min to apply the second insulating barrier Photosensitive polyimides in 240 ℃ convection oven again, and thickness is 1.5 μ m.In 190 ℃ convection oven, toast 20min.The Photosensitive polyimides is carried out photoetching formation and the transparency conducting layer vertical element parallel to each other of quadrature mutually, and wherein developing time is 40s, and live width is that 20 μ m, lines gap are 0.25mm.In 180 ℃ convection oven, toast 10min once more.Figure with the Photosensitive polyimides is that mask develops to ground floor plain edition polyimide film, prolonging developing time makes the edge of ground floor plain edition polyimides than the inside 2 μ m of contraction in the edge of second layer Photosensitive polyimides, developing time is 45s, live width is that 16 μ m, lines gap are 0.254mm, so obtain down trapezoidal insulated column figure.At last whole figure is toasted once more, temperature is 250 ℃, time 20min.After the preparation of insulated column figure is finished, continue evaporation organic layer and metal level.Organic layer is successively by CuPc, NPB and Alq
3Form, thickness is respectively 7nm, 35nm and 40nm.Metal level is made up of Mg-Ag alloy and Ag successively, and thickness is respectively 150nm and 50nm.The evaporation speed of organic layer is 0.1nm/s, and the evaporation speed of Mg-Ag alloy and Ag is 0.6nm/s.The evaporation speed of organic layer is 0.1nm/s, and the evaporation speed of metal level is 0.6nm/s.It is 3V that device plays bright voltage, luminous even.
Embodiment two:
Sputter layer of transparent conducting film ITO on transparent glass substrate, thickness is 70nm, and square resistance is 60 Ω, and photoetching forms one group of vertical element parallel to each other, and live width is that 0.6mm, lines gap are 100 μ m.Rotation applies the first insulating barrier plain edition polyimides after acetone ethanol is cleaned, and thickness is 4 μ m, rotates behind the baking 30min to apply the second insulating barrier negative photoresist in 220 ℃ convection oven again, and thickness is 2.5 μ m.In 150 ℃ convection oven, toast 30min.Negative photoresist is carried out photoetching formation and the transparency conducting layer vertical element parallel to each other of quadrature mutually, and wherein developing time is 90s, and live width is that 100 μ m, lines gap are 0.6mm.In 160 ℃ convection oven, toast 20min once more.Figure with negative photoresist is that mask develops to ground floor plain edition polyimide film, prolonging developing time makes the edge of ground floor plain edition polyimides than the inside 15 μ m of contraction in the edge of second layer negative photoresist, developing time is 2min, live width is 70 μ m, lines gap 0.63mm, so obtain down trapezoidal insulated column figure.At last whole figure is toasted once more, temperature is 140 ℃, and the time is 40min.After the preparation of insulated column figure is finished, continue evaporation organic layer and metal level.Organic layer is successively by CuPc, NPB and Alq
3Form, thickness is respectively 25nm, 40nm and 70nm.Metal level is made up of LiF and Al successively, and thickness is respectively 0.5nm and 150nm.The evaporation speed of organic layer is 0.3nm/s, the evaporation speed 0.2nm/s of LiF, and the evaporation speed of Al is 1.2nm/s.It is 3.5V that device plays bright voltage, luminous even.
Embodiment three:
Sputter layer of transparent conducting film ITO on transparent glass substrate, thickness is 230nm, and square resistance is 10 Ω, and photoetching forms one group of vertical element parallel to each other, and live width is that 0.4mm, lines gap are 40 μ m.Rotation applies the first insulating barrier Photosensitive polyimides after acetone ethanol is cleaned, and thickness is 2 μ m, rotates behind the baking 50min to apply the second insulating barrier negative photoresist in 100 ℃ convection oven again, and thickness is 2 μ m.In 80 ℃ convection oven, toast 40min.Negative photoresist is carried out photoetching formation and the transparency conducting layer vertical element parallel to each other of quadrature mutually, and wherein developing time is 2min, and live width is that 40 μ m, lines gap are 0.4mm.In 110 ℃ convection oven, toast 25min once more.Figure with negative photoresist is that mask develops to ground floor Photosensitive polyimide film, prolonging developing time makes the edge of ground floor Photosensitive polyimides than the inside 5 μ m of contraction in the edge of second layer negative photoresist, developing time is 1min, live width is that 30 μ m, lines gap are 0.41mm, so obtain down trapezoidal insulated column figure.At last whole figure is toasted once more, temperature is 95 ℃, and the time is 30min.After the preparation of insulated column figure is finished, continue evaporation organic layer and metal level.Organic layer is successively by CuPc, NPB and Alq
3: DCM forms, and thickness is respectively 15nm, 40nm and 60nm.DCM is at Alq
3In doping be 8%.Metal level is made up of Mg-Ag alloy and Ag successively, and thickness is respectively 100nm and 70nm.The evaporation speed of organic layer is 0.4nm/s, and the evaporation speed of Mg-Ag alloy and Ag is 1nm/s.It is 4V that device plays bright voltage, luminous even.Sputter layer of transparent conducting film ZnO also can reach above-mentioned effect as first electrode on transparent glass substrate.
Claims (7)
1, a kind of preparation method of organic electroluminescence device is characterized in that this method may further comprise the steps:
(1) on transparency carrier the deposit transparent conductive film as first electrode of device, thickness is 20nm～250nm, the square resistance of conducting film is 5 Ω～70 Ω, on transparent conductive film, make one group of vertical element that is parallel to each other and separates then by lithography, the width that makes first electrode is 50 μ m～1.5mm, and the gap between the electricity level is 5 μ m～120 μ m;
(2) rotation simultaneously applies first insulating barrier on the gap between above-mentioned first electrode and the electricity level, and the thickness of first insulating barrier is 1 μ m～5 μ m, baking 10min～60min under 70 ℃～300 ℃;
(3) continue rotation on above-mentioned first insulating barrier and apply second insulating barrier, the thickness of second insulating barrier is 0.5 μ m～3 μ m, toasts 10min～60min down at 70 ℃～300 ℃;
(4) above-mentioned second insulating barrier is carried out photoetching, form and above-mentioned transparent first electrode vertical element a plurality of parallel to each other of quadrature mutually, wherein developing time is 30s～2min, the width that makes second insulating barrier is 5 μ m～120 μ m, the gap is 50 μ m～1.5mm, toasts 10min～40min down at 70 ℃～300 ℃;
(5) figure with above-mentioned second insulating barrier is a mask, first insulating barrier is developed, form and above-mentioned transparent first electrode vertical element a plurality of parallel to each other of quadrature mutually, developing time is 30s～2min, the edge that makes first insulating barrier is than the inside 1 μ m～20 μ m of contraction in the edge of second insulating barrier, obtain the up big and down small trapezoidal insulated column that falls, the width of insulated column is 3 μ m～110 μ m, the gap is 60 μ m～1.6mm, above-mentioned two insulating barriers are toasted, baking temperature is 70 ℃～300 ℃, and the time is 10min～60min;
(6) on above-mentioned second insulating barrier and removed evaporation organic layer on the transparent conductive film of two insulating barriers and the transparent conductive film lines gap, the evaporation speed of organic membrane is 0.1nm/s～0.5nm/s;
(7) evaporated metal layer is as second electrode of device on above-mentioned organic layer, and the evaporation speed of metal film is 0.2nm/s～1.5nm/s, is organic electroluminescence device.
2, the method for claim 1 is characterized in that wherein said first electrode is tin indium oxide or zinc oxide.
3, the method for claim 1 is characterized in that wherein said first insulating barrier is plain edition polyimides or Photosensitive polyimides.
4, the method for claim 1 is characterized in that wherein said second insulating barrier is Photosensitive polyimides or negative photoresist.
5, the method for claim 1 is characterized in that wherein said organic layer is a single layer structure, and material is 8-hydroxyquinoline aluminum or N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4,4-diamines.
6, the method of claim 1, it is characterized in that wherein said organic layer is a sandwich construction, material is followed successively by ketone peptide cyanogen, N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4,4-diamines and 8-hydroxyquinoline aluminum or be followed successively by ketone peptide cyanogen, N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4, the 4-diamines, 8-hydroxyquinoline aluminum: 4-methylene dicyanoethyl-2-methyl-6-(p-dimethylamino styryl)-4H-pyrans, ketone peptide cyanogen thickness is 5nm～30nm, N, N '-two-(1-naphthyl)-N, N '-diphenyl-1,1-xenyl-4,4-diamines thickness is 30nm～70nm, the 8-hydroxyquinoline aluminum thickness is 30nm～80nm, and 4-methylene dicyanoethyl-2-methyl-6-(p-dimethylamino styryl)-doping of 4H-pyrans in 8-hydroxyquinoline aluminum is 1%～10%.
7, the method for claim 1, it is characterized in that wherein said metal level is Mg-Ag alloy and Ag or LiF and Al, Mg-Ag alloy thickness is 80nm～200nm, and the Ag thickness is 20nm～100nm, the LiF thickness is 0.2nm～1nm, and the Al thickness is 100nm～200nm.
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| CN1308481C (en) * | 2003-02-20 | 2007-04-04 | 东北先锋电子股份有限公司 | Mask for vacuum deposition and organic el display panel manufactured by using the same |
| CN1322600C (en) * | 2002-03-11 | 2007-06-20 | 三洋电机株式会社 | Optical element and its making method |
| CN100372443C (en) * | 2004-07-06 | 2008-02-27 | 胜华科技股份有限公司 | Method for making display |
| CN100461488C (en) * | 2002-05-03 | 2009-02-11 | 乐金显示有限公司 | Organic electroluminescence display device and its mfg. method |
| CN100496175C (en) * | 2005-11-24 | 2009-06-03 | 中国科学院微电子研究所 | Preparation method of silicon-based organic light-emitting micro-display metal anode and cathode isolation column |
| US7837528B2 (en) | 2002-11-29 | 2010-11-23 | Samsung Mobile Display Co., Ltd. | Evaporation mask, method of fabricating organic electroluminescent device using the same, and organic electroluminescent device |
| CN102222684A (en) * | 2011-06-30 | 2011-10-19 | 信利半导体有限公司 | Organic electroluminescent display and manufacture method thereof |
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