CN1642376A - Organic electroluminiscence element and its making method - Google Patents
Organic electroluminiscence element and its making method Download PDFInfo
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- CN1642376A CN1642376A CN 200410001060 CN200410001060A CN1642376A CN 1642376 A CN1642376 A CN 1642376A CN 200410001060 CN200410001060 CN 200410001060 CN 200410001060 A CN200410001060 A CN 200410001060A CN 1642376 A CN1642376 A CN 1642376A
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Abstract
The invention discloses an organic electro-light emitting device and its preparing method. It at least comprises light-emitting layer as well as cathode layer and anode layer situated on and under the light -emitting layer, respectively, and the anode of the anode layer is silicon-made. Its preparing method includes the steps as follows: 1) making ohm contact metal at the back of the silicon; 2) then growing a cavity injection/control layer on the right side of the silicon plate with the ohm contact metal; 3) in turn vacuum-depositing a cavity transmission layer, a light-emitting layer, an electron transmission layer and an electron injection/control layer; 4) by template deposition method or deposition plus photoetching method, in turn preparing light transmitting cathode and thick cathode on the electron injection/control layer; 5) preparing device passivation protective membrane on the light transmitting cathode and the thick cathode. It can be widely applied to the fields of video digital display, instrument monitoring, advertisement, etc. It can also implement microdisplay, personal 'watching', and other special requirements, thus used in the special fields of military, electronic game, etc.
Description
Technical field
The present invention relates to a kind of organic electroluminescence device and preparation method thereof in the luminescent device field.
Background technology
Organic light emission is (Appl.Phys.Lett.51,913) after obtaining important breakthrough in 1987, progressively possessed the big and high characteristics of efficient of brightness, satisfy the requirement of practicability substantially.At present, common organic electroluminescence device is (Materials Science and Engineering R 39 (2002) 143-222) of substrate with the conductive transparent material.
Silicon is the microelectronics critical material, but because silicon has indirect forbidden band structure, and luminous efficiency is more much lower than direct energy-gap semiconductor, therefore is considered to not be suitable for the light source that plays a crucial role in the photonic propulsion for a long time.Nineteen ninety Canham (Appl.Phys.Lett.57,1046) starts the silicon base luminescence research boom after finding the photoluminescence of porous silicon room temperature high light in the international coverage.But the electroluminescent efficient of silicon-based nano silicon/oxidative silicon composite construction is generally also lower at present, also has quite distance (Current Opinion in Solids State ﹠amp from practicality; Material Science, 7,97 (2003)).
The innovation and creation content
The purpose of this invention is to provide the higher organic electroluminescence device of a kind of luminous efficiency.
Organic electroluminescence device provided by the present invention comprises luminescent layer at least, and lays respectively at described luminescent layer cathode layer and anode layer up and down, and the anode of described anode layer is a silicon.
In order to improve the ability that electrode injects electronics and hole, improve luminous efficiency, described organic electroluminescence device also comprises electron transfer layer and hole transmission layer; Described electron transfer layer is between described luminescent layer and negative electrode, and described hole transmission layer is between described luminescent layer and anode.
In order to improve the stability of described organic EL device, also has device passivation protection film on the cathode layer of described organic EL device.Described device passivation protection mould can be the inorganic or organic transparent material with passivation, strengthens the plasma chemical deposition as utilizing, the SiO of any conventional method growth such as low temperature sputter or electron beam evaporation
2, Si
3N
4, MgF, or the polycarbonate of chemical method preparation, epoxy resin.
Wherein, above-mentioned anode layer also comprises being connected to described silicon anode hole injection/key-course and metal ohmic contact up and down except that comprising the silicon anode; Above-mentioned cathode layer comprises electronics injection/key-course, transparent cathode and thick negative electrode, wherein, described thick negative electrode and electronics injection/key-course be connected to the top of described transparent cathode and below.
Described silicon anode is a p type silicon chip, wherein, and resistance or low-resistance p type silicon chip or p/p in being preferably
+Silicon epitaxial wafer; Described metal ohmic contact is an aluminium; Described hole injection/key-course can be by SiO
2(1-10nm) or/and CuPc (5-100nm) composition.
The thickness of described electronics injection/key-course is the 0.1-3.0 nanometer, and its composition material can be alkali metal fluoride, as lithium fluoride, and cesium fluoride; Described transparent cathode can be: gross thickness is the semi-transparent metals single or multiple lift film of 5-40 nanometer, as be aluminium, calcium, the monofilm of low workfunction metal such as magnesium or ytterbium, or be aluminium, calcium, the alloy monofilm that noble metals such as low workfunction metal such as magnesium or ytterbium and silver or gold are formed, or aluminium, calcium, the multilayer film that noble metals such as low workfunction metal such as magnesium or ytterbium and silver, gold constitute, or the multilayer film of the alloy of low workfunction metal and noble metal and noble metal formation; Or thickness is the oxidic transparent conductive layers of 0.1-10 micron, as ITO, and In
2O
3, SnO
2Or ZnO etc.
When described transparent cathode is an aluminium, when calcium, alloy monofilm that low workfunction metal such as magnesium or ytterbium and noble metals such as silver or gold are formed, the weight ratio of described low workfunction metal and noble metal is 5-20: 1.
Described thick negative electrode is to combine good thick metal with its below transparent cathode, can be any geometry, and as circle or pectination, thickness can be the 0.1-40 micron, as titanium/golden composite material.Described thick negative electrode is connected with transparent cathode, and the former is used for pressure welding lead and introduce electric current, and is light tight.
The thickness of described luminescent layer can be the 1-100 nanometer; The material of described luminescent layer can be p-phenylene vinylene (PPV), polythiophene, polyhenylene, macromolecular materials such as kayexalate, Sodium Polyacrylate, poly-amino ethene and derivative thereof; Also can be Eu, Tb, Ru, Nd, Er and Phen, the metal complex that triphenylphosphinc oxide etc. are formed; Or oxine aluminium (AlQ), cumarin, small molecule materials such as rubrene.
The thickness of described hole transmission layer can be the 1-150 nanometer; The composition material of described hole transmission layer can be NPB (N, N '-diphenyl-N-N ' two (1-naphthyl)-1,1 ' diphenyl-4,4 '-diamines) or TPD (N, N '-diphenyl-N-N ' two (3-aminomethyl phenyl)-1,1 ' diphenyl-4,4 '-diamines) etc. aromatic amine compounds; The thickness of described electron transfer layer can be the 1-150 nanometer; The material of described electron transfer layer can be some metallo-chelates, as oxine aluminium and 1,3, and the derivative of 4-oxadiazoles, as connecting benzene-to tert-butyl benzene-1,3, the 4-oxadiazoles, and 1,2,4 ,-triazole.
It is the preparation method of the organic electroluminescence device of anode with silicon that second purpose of the present invention provides a kind of.This method may further comprise the steps:
1) makes metal ohmic contact at the silicon chip back side;
2) at the described positive growth of the silicon chip hole injection/key-course that has prepared metal ohmic contact of step 1);
3) in step 2) vacuum deposition hole transmission layer successively on the injection/key-course of described hole, luminescent layer, electron transfer layer, electronics injection/key-course;
4) on the described electronics injection/key-course of step 3), prepare transparent cathode and thick negative electrode with template sedimentation or the method that adds photoetching with deposit successively;
5) fabricate devices passivation protection film on described transparent cathode of step 4) and thick negative electrode.
Wherein, step 1), 2) and 5) all can finish according to a conventional method.
In actual applications, as the case may be, can omit the hole injection/key-course 3 in the above-mentioned organic electroluminescence devices, also can be with hole transmission layer 4 and luminescent layer 5 or luminescent layer 5 and electron transfer layer 6 synthetic one decks, they all can be with reference to method for preparing.
The principle of luminosity of organic electroluminescence device shown in Figure 1 is: electronics is injected into electron transfer layer 6 from negative electrode 9 and 8 through electronics injection/key-course 7, enters the lowest unoccupied molecular orbital of luminescent layer 5 then; The hole is injected into hole transmission layer 4 from silicon substrate 2 through hole injection layer 3, enters the highest occupied molecular orbital of luminescent layer 5 then.Be injected into the electronics of luminescent layer and hole (forming or do not form exciton) radiation recombination and luminous.Emission wavelength depends on the energy level difference between lowest unoccupied molecular orbital and the highest occupied molecular orbital.
The present invention combines silicon and luminous organic material, be deposited on luminous organic material on the silicon anode rather than on the transparent conductive anode, made full use of the advantage of silicon and luminous organic material, realized high efficiency silica-based electroluminescence, laid the first stone for silicon based opto-electronics is integrated.Can make at present with silicon is that the performance of organic electroluminescence device of anode is near being the performance of the electroluminescent device of anode with the conductive transparent material.Organic electroluminescence device of the present invention can be widely used in fields such as digital video demonstration, instruments monitor, advertisement; Also can realize little demonstration, (Microdisplay), specific (special) requirements such as " seeing " with oneself, thus be used in special dimensions such as military affairs, electronic game.
Description of drawings
Fig. 1 be of the present invention be the organic electroluminescence device structural representation of anode with silicon
Embodiment
According to following prepared ten layers of organic electroluminescence device as shown in Figure 1:
1) press standard technology cleaning silicon chip 2, make metal ohmic contact 1 as follows at silicon chip 2 back sides: with vacuum deposition method at the back side of silicon evaporation layer of metal aluminium, then under nitrogen protection in annealing furnace, with 500 ℃ heat-treated 10 minutes.
2) utilize autoxidation, thermal oxidation or vacuum deposition method growing and preparing hole injection/key-course 3 in silicon substrate 2 fronts;
3) vacuum deposition hole transmission layer 4 successively on hole injection/key-course 3, luminescent layer 5, electron transfer layer 6, electronics injection/key-course 7;
4) on electronics injection/key-course 7, prepare transparent cathode 8 and thick negative electrode 9 successively with the template sedimentation;
5) on thick negative electrode 9, utilize the low temperature sputter to prepare Si
3N
4As device passivation protection film 10.
Six layers of organic electroluminescence device of embodiment 2, green light
Six layers of organic electroluminescence device that prepare following green light with reference to the method for embodiment 1: silicon chip 2 is p/p
+Silicon epitaxial wafer, back side metal ohmic contact 1 is an aluminium; Hole transmission layer 4 is the NPB of about 70 nanometer thickness; Electron transfer layer 6 and luminescent layer 5 unite two into one, and are the AlQ of about 70 nanometer thickness; Electronics injection/key-course 7 is the LiF layer of about 0.2 nanometer thickness; Transparent cathode 8 is the aluminium lamination of about 15 nanometer thickness; Save layer 3.This device green light.Luminous power efficiency is about 0.1-1%.
Six layers of organic electroluminescence device of embodiment 3, green light
Six layers of organic electroluminescence device that prepare following green light with reference to the method for embodiment 1: silicon chip 2 is low-resistance p type silicon, and back side metal ohmic contact 1 is an aluminium; Hole transmission layer 4 is the NPB (N, N '-diphenyl-N-N ' two (1-naphthyl)-1,1 ' diphenyl-4,4 '-diamines) of about 70 nanometer thickness; Electron transfer layer 6 and luminescent layer 5 are combined into one deck, are the AlQ of about 70 nanometer thickness; Electronics injection/key-course 7 is the LiF layer of about 0.2 nanometer thickness; Transparent cathode 8 is the aluminium of about 2 nanometer thickness and the gold double-deck (the gold layer is on aluminium lamination) of 15 nanometer thickness; Save layer 3.This device green light.Luminous power efficiency is 0.1-1%.
Method with reference to embodiment 1 prepares following seven layers of organic electroluminescence device that glow: silicon chip 2 is middle resistance silicon chip, and back side metal ohmic contact 1 is an aluminium; Hole transmission layer 4 is the NPB of about 50 nanometer thickness; Electron transfer layer 6 is the AlQ of about 50 nanometer thickness; Luminescent layer 5 is europium and the trifluoroacetyl thiophene acetone and second ligand 1, the complex (Eu (TTA) that 10 Phens form
3Phen), thick about 30 nanometers; Electronics injection/key-course 7 is the lithium fluoride layer of thick about 0.2 nanometer; Transparent cathode 8 is the aluminium of about 2 nanometer thickness and the gold double-deck (the gold layer is on aluminium lamination) of 15 nanometer thickness.This device has independently metal complex luminescent layer, glows.Luminous power efficiency is 0.01-0.1%.
Eight layers of organic electroluminescence device of embodiment 5, the green glow that turns blue
Eight layers of organic electroluminescence device that prepare the following green glow that turns blue with reference to the method for embodiment 1: silicon chip 2 is middle resistance p type silicon chip, and back side metal ohmic contact 1 is an aluminium; Hole injection/key-course 3 is the thick SiO of about 10nm
2Layer; Hole transmission layer 4 is the NPB of about 50 nanometer thickness; Electron transfer layer 6 is the AlQ of about 50 nanometer thickness; Luminescent layer 5 is the AlQ of 1% cumarin (Kui acridone Quinacridone QA) that mixes, thick about 40 nanometers; Electronics injection/key-course 7 is the lithium fluoride layer of thick approximately 0.2 nanometer; Transparent cathode 8 is the aluminium silver alloy (10: 1, weight ratio) of about 20 nanometer thickness.This device has independently organic molecule luminescent layer, and green glow turns blue.Luminous power efficiency is 0.1-1%.
Eight layers of organic electroluminescence device of embodiment 6, jaundice light
Eight layers of organic electroluminescence device that prepare following jaundice green glow with reference to the method for embodiment 1: silicon chip 2 is middle resistance p type silicon chip, and back side metal ohmic contact 1 is an aluminium; Hole injection/key-course 3 is the thick SiO of about 10nm
2 Hole transmission layer 4 is the NPB of about 40 nanometer thickness; Electron transfer layer 6 is the AlQ of about 40 nanometer thickness; Luminescent layer 5 is thick about 60 nanometers of p-phenylene vinylene; Electron injecting layer 7 is the lithium fluoride layer of thick approximately 0.2 nanometer; Transparent cathode 8 is the magnesium silver alloy (10: 1) of about 20 nanometer thickness.This device has independently polymeric luminescence layer, jaundice.Luminous power efficiency is 0.01-0.1%.
Eight layers of organic electroluminescence device of embodiment 7, green light
Eight layers of organic electroluminescence device that prepare following green light with reference to the method for embodiment 1: silicon chip 2 is p/p
+Silicon epitaxial wafer, back side metal ohmic contact 1 is an aluminium; Hole injection/key-course 3 is the thick SiO of about 10nm
2 Hole transmission layer 4 is the NPB of about 40 nanometer thickness; Electron transfer layer 6 is the AlQ of about 40 nanometer thickness; Luminescent layer 5 is phosphor material precious metal iridium complex Ir (ppy)
3(its molecular formula is: tris (2-phenylpyridine) iridium), and thick about 60 nanometers; Electron injecting layer 7 is the lithium fluoride layer of thick approximately 0.2 nanometer; Transparent cathode 8 is the magnesium silver alloy (10: 1, weight ratio) of about 20 nanometer thickness.This device has independently phosphorescence luminescent layer, green light.Luminous power efficiency is 1-10%.
Eight layers of organic electroluminescence device of embodiment 8, green light
Eight layers of organic electroluminescence device that prepare following green light with reference to the method for embodiment 1: silicon chip 2 is p/p
+Silicon epitaxial wafer, back side metal ohmic contact 1 is an aluminium; Hole injection/key-course 3 is the thick SiO of about 10 nm
2 Hole transmission layer 4 is the NPB of about 40 nanometer thickness; Electron transfer layer 6 is the AlQ of about 40 nanometer thickness; Luminescent layer 5 is phosphor material precious metal iridium complex (Ir-2h) (its molecular formula is: fac-tris[fluoro-2-(5-trifluoromethyl-2-pyridinyl) phenyl-C, N] iridium), thick about 60 nanometers; Electron injecting layer 7 is the lithium fluoride layer of thick approximately 0.2 nanometer; Transparent cathode 8 is the aluminium silver alloy (10: 1, weight ratio) of about 20 nanometer thickness.This device has independently phosphorescence luminescent layer, green light.Luminous power efficiency is 1-10%.
Claims (10)
1, a kind of organic electroluminescence device which comprises at least luminescent layer, and lays respectively at described luminescent layer cathode layer and anode layer up and down, and it is characterized in that: the anode of described anode layer is a silicon.
2, organic electroluminescence device according to claim 1 is characterized in that: described organic electroluminescence device also comprises electron transfer layer and hole transmission layer; Described electron transfer layer is between described luminescent layer and cathode layer, and described hole transmission layer is between described luminescent layer and anode layer.
3, organic electroluminescence device according to claim 1 and 2 is characterized in that: the cathode layer of described organic electroluminescence device is provided with device passivation protection film.
4, organic electroluminescence device according to claim 3 is characterized in that: described anode layer also comprises and is connected to described silicon anode hole injection/key-course and metal ohmic contact up and down; Described cathode layer comprises electronics injection/key-course, transparent cathode and thick negative electrode, wherein, described thick negative electrode and electronics injection/key-course be connected to the top of described transparent cathode and below.
5, organic electroluminescence device according to claim 4 is characterized in that: described silicon substrate is a p type silicon chip, wherein, and resistance or low-resistance p type silicon chip or p/p in being preferably
+Silicon epitaxial wafer; Described metal ohmic contact is an aluminium; The thickness of described hole injection/key-course is the 1-100 nanometer, and composition material is SiO
2, CuPc.
6, organic electroluminescence device according to claim 4 is characterized in that: the thickness of described electronics injection/key-course is the 0.1-3.0 nanometer, and its composition material is an alkali metal fluoride; Described transparent cathode is that gross thickness is the semi-transparent metals single or multiple lift film of 5-40 nanometer, or thickness is the oxidic transparent conductive layers of 0.1-10 micron; Described thick negative electrode is that thickness is the metal film of 0.1-40 micron, and described metal film is titanium/golden composite material.
7, organic electroluminescence device according to claim 6, it is characterized in that: the composition material of described semi-transparent metals monofilm is the alloy of low workfunction metal or described low work function and noble metal, and the composition material of described semi-transparent metals multilayer film is the alloy and the noble metal of low workfunction metal, low workfunction metal and noble metal; Described low workfunction metal is an aluminium, calcium, magnesium or ytterbium; Described noble metal is a silver or golden; Described oxide is ITO, In
2O
3, SnO
2Or ZnO.
8, organic electroluminescence device according to claim 1 is characterized in that: the thickness of described luminescent layer is the 1-100 nanometer; The composition material of described luminescent layer is p-phenylene vinylene (PPV), polythiophene, polyhenylene, kayexalate, Sodium Polyacrylate, poly-amino ethene and derivative thereof; Or Eu, Tb, Ru, Nd, Er and Phen, the metal complex that triphenylphosphinc oxide is formed; Or oxine aluminium (AlQ), cumarin, rubrene.
9, organic electroluminescence device according to claim 2 is characterized in that: the thickness of described hole transmission layer is the 1-100 nanometer, and its composition material is NPB or TPD; The thickness of described electron transfer layer is the 1-100 nanometer, and its composition material is oxine aluminium and 1,3, and the derivative of 4-oxadiazoles is wherein said 1,3, and the derivative of 4-oxadiazoles is for connecting benzene-to tert-butyl benzene-1,3,4-oxadiazoles and 1,2,4 ,-triazole.
10, a kind of method for preparing the described organic electroluminescence device of claim 4 may further comprise the steps:
1) makes metal ohmic contact at the silicon chip back side;
2) at the described positive growth of the silicon chip hole injection/key-course that has prepared metal ohmic contact of step 1);
3) in step 2) vacuum deposition hole transmission layer successively on the injection/key-course of described hole, luminescent layer, electron transfer layer, electronics injection/key-course;
4) on the described electronics injection/key-course of step 3), prepare transparent cathode and thick negative electrode with template sedimentation or the method that adds photoetching with deposit successively;
5) fabricate devices passivation protection film on described transparent cathode of step 4) and thick negative electrode.
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102064284A (en) * | 2010-12-01 | 2011-05-18 | 郑州大学 | Organic electroluminescent device |
| CN101436636B (en) * | 2008-12-16 | 2011-05-25 | 中国科学院电工研究所 | Transparent conductive cathode contact structure for n type silicon |
| CN102881837A (en) * | 2012-09-28 | 2013-01-16 | 京东方科技集团股份有限公司 | Packaging structure and packaging method for light emitting device and display device |
| CN103258960A (en) * | 2013-05-10 | 2013-08-21 | 重庆大学 | Preparation method of organic thin film transistor |
-
2004
- 2004-01-18 CN CN 200410001060 patent/CN1642376A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101436636B (en) * | 2008-12-16 | 2011-05-25 | 中国科学院电工研究所 | Transparent conductive cathode contact structure for n type silicon |
| CN102064284A (en) * | 2010-12-01 | 2011-05-18 | 郑州大学 | Organic electroluminescent device |
| CN102881837A (en) * | 2012-09-28 | 2013-01-16 | 京东方科技集团股份有限公司 | Packaging structure and packaging method for light emitting device and display device |
| CN102881837B (en) * | 2012-09-28 | 2015-03-11 | 京东方科技集团股份有限公司 | Packaging structure and packaging method for light emitting device and display device |
| CN103258960A (en) * | 2013-05-10 | 2013-08-21 | 重庆大学 | Preparation method of organic thin film transistor |
| CN103258960B (en) * | 2013-05-10 | 2015-10-21 | 重庆大学 | A kind of preparation method of OTFT |
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