CN103337585A - Solid illuminant total internal reflection light lead-out method based on TiO2 nano particle porous membrane - Google Patents
Solid illuminant total internal reflection light lead-out method based on TiO2 nano particle porous membrane Download PDFInfo
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Abstract
The invention discloses a method for improving the luminous efficiency of a solid illuminant by utilizing a near-field effect between a porous TiO2 nano particle multilayer membrane and total internal reflection light of a luminous surface of the solid illuminant. The method comprises the following steps that (a) the solid illuminant is fixed on a base; (b) Ti atoms generated by an atomizer grow into Ti clusters in inert gas; the Ti clusters form Ti nano particle beams through a nozzle and collimators; and (c) nano particles conduct oblique incidence deposition on the luminous surface of the solid illuminant; a self-masking effect in the oblique incidence deposition results in forming of a porous structure; oxygen is filled in a high vacuum deposition chamber during deposition; the Ti nano particles are oxidized into TiO2 nano particles; or the TiO2 nano particles reach a required coverage rate and the required layer number by adopting a manner of alternate deposition/oxidation. The method has the characteristics that the method is high in controllability and high in efficiency, has high compatibility with a luminous device fabrication technology, has a small influence on the luminous characteristic of the solid illuminant, and can be combined with a universal micron-sized rough luminous reinforcement structure.
Description
One, technical field
The present invention relates to fields such as nano material, light emitting semiconductor device, photoelectron technology, relate in particular to a kind of based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane.
Two, background technology
Solid-state light emitters (as: semiconductor light-emitting-diode (LED), organic luminorphor) can directly be converted into visible light with electric energy, development in recent years is rapid, because its special advantage has obtained at aspects such as various colorful display screens, decorative lamp, indicator light, white-light illuminating lamps using widely, and following prospect is more wide.Yet the efficient of Sony ericsson mobile comm ab is subjected to the restriction of many-sided factor, does not reach dreamboat so far yet, and leeway still is greatly improved.
The photoelectric conversion efficiency of solid-state light emitters is determined jointly by internal quantum efficiency and light extraction efficiency.Development along with the semiconductor fabrication technology, the improvement of internal quantum efficiency has obtained bigger progress, near theoretical limit (K. Y. Zang, S. J. Chua, J. H. Teng, N. S. S. Ang, A. M. Yong, and S. Y. Chow. Appl. Phys. Lett. 92,243126 (2008)).What therefore at present influence Sony ericsson mobile comm ab efficient mainly is light extraction efficiency.Because the refractive index of solid-state light emitters and air there are differences, cause its luminous a big chunk in the interface of luminous element and air experiences total internal reflection, in turning back in the luminous element, final loss is heat, this makes luminous efficiency not improve on the one hand, also cause device temperature to raise on the other hand, influence the life-span.Therefore, reduce total internal reflection loss for the efficient that improves Sony ericsson mobile comm ab and stable significant.Adopt rough surface (S. J. Chang, C. F. Shen, W. S. Chen, C. T. Kuo, T. K. Ko, S. C. Shei, and J. K. Sheu, Appl. Phys. Lett. 91 (2007) 013504), the side that tilts, and prepare photonic crystal (K. McGroddy, A. David, E. Matioli at exiting surface, M. Iza, S. Nakamura et al. Appl. Phys. Lett. 93,103502 (2008)) etc. nanostructure, all be proved to be effectively to draw the method for total internal reflection light.Photonic crystal can improve the efficient of Sony ericsson mobile comm ab to a certain extent, but because the processing technology of photonic crystal is usually directed to dry etching epitaxial loayer (can with reference to Chinese patent literature CN00123550.8 " tool roughed interface light-emitting component and preparation method thereof "), may cause damage to active area, thereby reduction even counteracting are to the effect of luminous enhancing.Method for coarsening surface mainly contains wet etching and dry etching, and there is significant disadvantages in wet etching, because the isotropism of wet etching is easy to produce undercutting and crosses erosion, the size of alligatoring and the degree of depth are subjected to certain restriction (usually less than 100nm); Same dry etching also may cause the decline of Sony ericsson mobile comm ab electrical properties.
Recently, people such as Periyayya Uthirakumar use chemical method to prepare the ZnO nano particle and then are spin-coated on the ITO transparency conducting layer of LED surface, nano particle has scattering process to total internal reflection light, part total internal reflection light becomes emergent light under the scattering of ZnO nano particle, can improve the LED luminous efficiency more than 10%.It is insecure that yet the ZnO nano particle that is spin-coated on the LED surface is combined with substrate, and have problems such as spin coating is inhomogeneous large-area the time.
Three, summary of the invention
1. goal of the invention
The purpose of this invention is to provide a kind of based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane, this method have can not damage to the electric property of Sony ericsson mobile comm ab, can make that its luminous efficiency is improved significantly utilizes nanometer particle beam to be deposited on the device exiting surface to prepare porous TiO
2The method of nanostructure is in order to effectively to draw total internal reflection light.The present invention can be used as replenishing of existing total internal reflection light extracting method such as surface roughening.
2. technical scheme
The present invention utilizes gas phase nano cluster line depositing system to produce nanometer particle beam.Air accumulation method cluster beam source 2 is connected on the vacuum chamber 7, cluster beam source 2 is made of atomizer 3 and condensation chamber 5, vacuum chamber 7 is separated by collimater 6 and is first order difference vacuum system 11 and second level difference vacuum system 12, and the two-stage vacuum system is vacuumized by mechanical pump, lobe pump and molecular pump respectively.Pedestal 10 is arranged in high vacuum settling chamber 9, atom nucleation in condensation chamber 5 inert gases 1 that atomizer 3 by in the air accumulation method cluster beam source 2 produces formation cluster of growing up, cluster is successively through nozzle 4 and the collimater 6 final nanometer particle beams 8 that form collimation, 8 pairs of nanocluster lines are positioned at the solid-state light emitters oblique incidence deposition on the pedestal 10, and nano particle has caused the formation of porous nano particle multilayer film from masking effect in the deposition process.Because size and the angle of deposit of nano particle can be regulated very easily in this method, and then porosity also can conveniently be regulated.Thereby the effect of the near field of nano particle perforated membrane and solid-state light emitters exiting surface total internal reflection light improves the light extraction efficiency that its light extraction efficiency improves solid-state light emitters.Therefore, this method provides that a kind of controllability is strong, technology is simple, high efficiency, strong to solid-state light emitters adaptability, with compatible strong, little to the influence of the solid-state light emitters characteristics of luminescence, the method that can strengthen the raising solid-state light emitters light extraction efficiency of structure and usefulness with the coarse bright dipping of general micron order of luminescent device preparation technology.
The operation principle of this method is: utilize magnetron sputtering or arc discharge to produce high density atom gas, carrying out just through the air accumulation process in cluster condensation chamber argon gas buffer gas, one-step growth forms nanocluster, form the nanometer particle beam of collimation again through the difference vacuum system, oblique incidence is deposited on the solid-state light emitters exiting surface then, the nano particle that the deposition initial stage arrives light output surface provides mask body for the nano particle that arrives afterwards, follow-up nano particle can't arrive the formed shadow region of mask body, along with the increase of sedimentation time, the particle membrane that is deposited on substrate surface shows as the space loose structure.The pore size of the how empty film of nano particle and porosity are determined by parameters such as incident nano-particles size and oblique incidence angle.Formed porous TiO
2Nanoparticulate thin films is scattering total internal reflection light effectively, because when the light experiences total internal reflection, on reflecting surface, also there is the evanescent wave of propagating along the surface simultaneously, evanescent wave is converted into the light radiation in far field by the how empty film of nano particle, reduce complete radiative intensity simultaneously, can be in order to improve the light extraction efficiency because of the lower solid-state light emitters of total internal reflection loss efficient.
Based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane, its preparation process is as follows:
(a) solid-state light emitters is fixed on the rotatable substrate pedestal 10 in the high vacuum settling chamber 9 of cluster line gas-phase deposition system, the exiting surface of luminous element is towards the line incident direction.
(b) air accumulation method cluster beam source 2 is connected on the vacuum chamber 7, and air accumulation method cluster beam source 2 adopts the air accumulation method to produce the cluster line.Utilize the mechanical pump of extract system, lobe pump and molecular pump vacuumize cluster line depositing system, in condensation chamber 5, feed 50 ~ 500Pa inert gas 1, produce high density Ti atom by atomizer 3, Ti atom nucleating growth in inert gas 1 forms the Ti cluster, by first order difference vacuum system 11 the Ti cluster in the condensation chamber 5 is ejected in the vacuum chamber 7 through nozzle 4 with inert gas, form Ti cluster line, by second level difference vacuum system 12 Ti cluster line is entered in the high vacuum settling chamber 9 through first collimater 6 and second collimater 6, form the nanocluster line 8 of high orientation;
(c) pedestal 10 in the rotation high vacuum settling chamber 9 makes 8 one-tenths 0 °～85 ° angles of solid-state light emitters light output surface normal direction and nanocluster line, utilize the generation of oblique incidence deposition from masking effect, the Ti nanoparticulate thin films of formation porous;
(d) in deposition process, feed the oxygen of 10 ~ 50Pa in the high vacuum settling chamber 9, make the Ti nano particle be oxidized to TiO
2Nano particle, or the mode that adopts deposition/oxidation to hocket earlier at vacuum condition deposit one deck Ti nano particle, stop deposition then, and the aerating oxygen oxidation extracts oxygen after finishing oxidation, the continuation vacuum moulding machine, and the deposition/oxidation cycle by such makes TiO
2Nano particle reaches required coverage rate and the number of plies at the solid-state light emitters light output surface, stops deposition.
Solid-state light emitters described in above-mentioned preparation method's step a is the Organic Light Emitting Diode of GaN base, GaP light-emitting diode or various emission visible lights.
Atomizer (3) described in above-mentioned preparation method's step b is to realize by magnetron sputtering or arc discharge.
The size of particle in the nanometer particle beam (8) described in above-mentioned preparation method's step b is controlled TiO by the air pressure that the distance between change atomizer (3) and the nozzle (4) or change charge into inert gas (1)
2The diameter of nano particle is 5 ~ 100nm.
Depositing in oblique incidence described in above-mentioned preparation method's step c regulated the porosity characteristic of nanoparticulate thin films by the angle of oblique incidence deposition, regulates TiO thereby reach
2The purpose of particle film effective refractive index, the adjustable range of nanometer particle beam oblique incidence angle are 0 °～85 °.
Preparation TiO described in above-mentioned preparation method's steps d
2The method of nano particle, in the mode that direct oxidation or deposition/oxidation hocket, the air pressure of aerating oxygen is 10 ~ 50Pa, oxidization time is 5min ~ 30min.
3. beneficial effect
The present invention proposes a kind of method of nano particle package assembly of new preparation controlled porosity, namely utilize cluster line technology to produce nanometer particle beam, the method by the oblique incidence deposition prepares porous nanometer structure at the solid-state light emitters exiting surface.Particularly, be by multilayer TiO in the preparation of the exiting surface of solid-state light emitters
2The film that the nano particle dense accumulation constitutes wherein is distributed with the hole of the 10-20 nanometer diameter that penetrates film, and duty ratio is 5%-30%.The method that this method has adopted the nanometer particle beam technology to be combined with the oblique incidence sedimentary facies, the nanostructure of preparing have with substrate characteristics such as be combined, chemical stability is good.The preparation technology of this nanostructure is also very simple simultaneously, because the size of nano particle can be regulated easily by changing correlated condition, angle of deposit also can be regulated arbitrarily, this just makes the present invention can prepare the nano particle structure of certain thickness and porosity according to the actual requirements, can also in quite wide scope, the refractive index to nanoparticulate thin films regulate by the adjusting of porosity simultaneously, to satisfy different application demands, this method is strong to solid-state light emitters adaptability, compatible strong with luminescent device preparation technology, little to the influence of the solid-state light emitters characteristics of luminescence, advantage such as can strengthen structure with the coarse bright dipping of general micron order and use.Therefore the invention provides a kind of controllability height, high efficiency, low cost, be easy to the method for preparing the nanometer diffusing structure of scale, be used for extracting solid-state light emitters total internal reflection light, improve the Sony ericsson mobile comm ab luminous efficiency.
Four, description of drawings
Fig. 1 (a): the nanocluster line depositing system structural representation that is used for realizing preparation method of the present invention.
Reference numeral:
The 1-inert gas;
2-air accumulation method cluster beam source;
3-atomizer (magnetron sputtering, arc discharge etc.);
The 4-nozzle;
The 5-condensation chamber;
The 6-collimater;
The 7-vacuum chamber;
8-nanocluster line;
9-high vacuum settling chamber;
The 10-pedestal;
11-first order difference vacuum system;
12-second level difference vacuum system;
(b): the oblique incidence of nanocluster line deposits from mask effect schematic diagram;
Fig. 2: (a) the total reflection prism surface does not deposit porous TiO
2Light path schematic diagram during nanoparticulate thin films; (b) the total reflection prism surface deposition porous TiO
2Light path schematic diagram during nanoparticulate thin films;
Reference numeral:
The 13-total reflection prism;
The ultraviolet-visible incident light that 14-is parallel;
15-total internal reflection light;
16-TiO
2Nanoparticulate thin films;
The 17-scattered light.
Fig. 3: porous TiO
2Nanoparticulate thin films surface and cross section scanning electron microscopy (SEM) photo;
Fig. 4: the relation that records scattered light and wavelength under total reflection condition according to Fig. 2 device;
Fig. 5: the TiO of the present invention's preparation
2Nanostructure LED and traditional LED electric current-intensity curve relatively;
Fig. 6: the TiO of the present invention's preparation
2Nanostructure LED and traditional LED voltage-to-current curve ratio are
Five, embodiment
Below respectively with at total reflection prism fully reflecting surface and GaN base blue-ray LED exiting surface depositing Ti O
2The nano particle porous membrane is example, and the TiO of this method preparation is described
2Nano particle porous membrane effectively scattering total internal reflection light also can effectively improve the solid-state light emitters light extraction efficiency.The basic procedure of this method:
1 one kinds of embodiment are based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane, its preparation methods steps is as follows:
(a) the semi-cylindrical total reflection prism with any surface finish is fixed on the rotatable pedestal 10, and fully reflecting surface is sealed in pedestal 10 in the high vacuum settling chamber 9 then towards the line incident direction, makes the prism fully reflecting surface be in the center of nanocluster line 8;
(b) air accumulation method cluster beam source 2 is connected on the vacuum chamber 7, air accumulation method cluster beam source 2 adopts the air accumulation method to produce the cluster line, utilize extract system mechanical pump, Lodz pump and molecular pump to vacuumize, the vacuum degree that makes high vacuum settling chamber 9 is 5 * 10
-4During Pa, charge into the argon gas 1 of 50Pa in the condensation chamber 5 of air accumulation method cluster beam source at inert gas entrance, under this air pressure, produce high density Ti atom gas by the atomizer 3 in the air accumulation method cluster beam source 2, Ti atom nucleating growth in argon gas forms the Ti cluster, by first order difference vacuum system 11 the Ti cluster in the condensation chamber 5 is ejected in the vacuum chamber 7 through nozzle 4 with argon gas, form Ti cluster line, making Ti cluster line by second level difference vacuum system 12 is that 2 millimeter first collimater 6 and second collimater 6 enter in the high vacuum settling chamber 9 through diameter, form the Ti nanometer particle beam 8 of high orientation, regulate input power, make Ti nanometer particle beam 8 deposition rates remain on about 1.2/s approximately;
(c) pedestal 10 in the rotation high vacuum settling chamber 9 makes the incidence angle of 8 one-tenth 85 ° of total reflection prism total reflection surface normal and Ti nanometer particle beams, controls the Ti nanometer particle beam total reflection prism total reflection surface is deposited;
(d) deposition/oxidation hockets in Chen Ji the process, and every deposition 2min control beam flow baffle plate interception line stops deposition, then 9 feeding 10Pa, the 99.99% pure O to the high vacuum settling chamber
2Oxidation 5min takes out O after oxidation is finished
2Recover high vacuum and continue deposition, total time reach 30min until deposition through 6 deposition/oxidation cycle cycles, stop to deposit, obtain porous TiO as shown in Figure 2
2The how empty film of nano particle.In order to measure the TiO of this method preparation
2Nanoparticulate thin films is to total internal reflection scattering of light efficient, and at first the parallel ultraviolet-visible incident light 14 that will produce with deuterium lamp-Halogen lamp LED is to become miter angle to be incident to total reflection prism with total reflection prism 13 fully reflecting surfaces, and as shown in Figure 2, there is not TiO in prism surface
2During nanoparticulate thin films 16, incident light 14 will namely all be converted into total internal reflection light 15 in prism fully reflecting surface experiences total internal reflection, because TiO
2The existence of nanoparticulate thin films 16, TiO
2The surface disappearance wave interaction that produces when nanoparticulate thin films 16 and experiences total internal reflection, the disappearance ripple finally is converted into far-field radiation, utilize the scattered light 17 of integrating sphere collection all directions and record scattered light spectrum with ultraviolet-visible spectrophotometer, scattered light light intensity and incident light beam intensity ratio can get scattering efficiency after, as shown in Figure 4, near GaN base blue-ray LED emission wavelength 450nm, utilize TiO
2The nano particle porous membrane can scattering about 4% total internal reflection light.
2 one kinds of embodiment are based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane, its preparation methods steps is as follows:
(a) just solid-state light emitters GaN base blue-ray LED is fixed on the rotatable substrate pedestal 10 in the high vacuum settling chamber 9 of cluster line gas-phase deposition system, the exiting surface of LED is towards the line incident direction, then pedestal 10 is sealed in the high vacuum settling chamber 9, makes the exiting surface of LED be in the center of nanocluster line 8;
(b) air accumulation method cluster beam source 2 is connected on the vacuum chamber 7, air accumulation method cluster beam source 2 adopts the air accumulation method to produce the cluster line, utilize extract system mechanical pump, Lodz pump and molecular pump to vacuumize, the vacuum degree that makes high vacuum settling chamber 9 is 1 * 10
-4During Pa, charge into the argon gas 1 of 180Pa in the condensation chamber 5 of air accumulation method cluster beam source at inert gas entrance, under this air pressure, produce high density Ti atom gas by the atomizer 3 in the air accumulation method cluster beam source 2, Ti atom nucleating growth in argon gas forms the Ti cluster, by first order difference vacuum system 11 the Ti cluster in the condensation chamber 5 is ejected in the vacuum chamber 7 through nozzle 4 with argon gas, form Ti cluster line, making Ti cluster line by second level difference vacuum system 12 is that 2 millimeter first collimater 6 and second collimater 6 enter in the high vacuum settling chamber 9 through diameter, form the Ti nanometer particle beam 8 of high orientation, regulate input power, make Ti nanometer particle beam 8 deposition rates remain on about 1.2/s approximately;
(c) pedestal 10 in the rotation high vacuum settling chamber 9 makes the incidence angle of 8 one-tenth 50 ° of solid-state light emitters light output surface normal and Ti nanocluster lines, controls Ti nanocluster line the LED light output surface is deposited;
(d) deposition/oxidation hockets in Chen Ji the process, and every deposition 2min control beam flow baffle plate interception line stops deposition, then 9 feeding 20Pa, the 99.99% pure O to the high vacuum settling chamber
2Oxidation 10min takes out O after oxidation is finished
2Recover high vacuum and continue deposition, total time reach 30min until deposition through 6 deposition/oxidation cycle cycles, stop to deposit, obtain porous TiO
2The how empty film of nano particle.TiO in the preparation of GaN base LED die surfaces
2The nano particle porous membrane, its surface topography and cross section pattern are as shown in Figure 3; TiO
2Nanostructure LED and traditional LED electric current-strength relationship curve contrast as shown in Figure 5, and current-voltage curve contrasts as shown in Figure 6.By Fig. 5 and Fig. 6 as can be known, the TiO of the present invention's preparation
2It is about 12% that the luminous efficiency of nanostructure GaN-LED has improved, TiO
2The existence of nanostructure does not produce any harmful effect to the electric property of LED.
3 one kinds of embodiment are based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane, its preparation methods steps is as follows:
(a) just solid-state light emitters GaP base green light LED is fixed on the rotatable substrate pedestal 10 in the high vacuum settling chamber 9 of cluster line gas-phase deposition system, the exiting surface of LED is towards the line incident direction, then pedestal 10 is sealed in the high vacuum settling chamber 9, makes the exiting surface of LED be in the center of nanocluster line 8;
(b) air accumulation method cluster beam source 2 is connected on the vacuum chamber 7, air accumulation method cluster beam source 2 adopts the air accumulation method to produce the cluster line, utilize extract system mechanical pump, Lodz pump and molecular pump to vacuumize, the vacuum degree that makes high vacuum settling chamber 9 is 1 * 10
-5During Pa, charge into the argon gas 1 of 250Pa in the condensation chamber 5 of air accumulation method cluster beam source at inert gas entrance, under this air pressure, produce high density Ti atom gas by the atomizer 3 in the air accumulation method cluster beam source 2, Ti atom nucleating growth in argon gas forms the Ti cluster, by first order difference vacuum system 11 the Ti cluster in the condensation chamber 5 is ejected in the vacuum chamber 7 through nozzle 4 with argon gas, form Ti cluster line, making Ti cluster line by second level difference vacuum system 12 is that 2 millimeter first collimater 6 and second collimater 6 enter in the high vacuum settling chamber 9 through diameter, form the Ti nanometer particle beam 8 of high orientation, regulate input power, make Ti nanometer particle beam 8 deposition rates remain on about 1.2/s approximately;
(c) pedestal 10 in the rotation high vacuum settling chamber 9 makes the incidence angle of 8 one-tenth 25 ° of solid-state light emitters light output surface normal and Ti nanocluster lines, controls Ti nanocluster line the LED light output surface is deposited;
(d) deposition/oxidation hockets in Chen Ji the process, and every deposition 2min control beam flow baffle plate interception line stops deposition, then 9 feeding 35Pa, the 99.99% pure O to the high vacuum settling chamber
2Oxidation 20min takes out O after oxidation is finished
2Recover high vacuum and continue deposition, total time reach 30min until deposition through 6 deposition/oxidation cycle cycles, stop to deposit, obtain porous TiO as shown in Figure 2
2The how empty film of nano particle.TiO in the preparation of GaN base LED die surfaces
2The nano particle porous membrane, the TiO of the present invention's preparation
2It is about 20% that the luminous efficiency of nanostructure GaP-LED has improved, TiO
2The existence of nanostructure does not produce any harmful effect to the electric property of LED.
4 one kinds of embodiment are based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane, its preparation methods steps is as follows:
(a) Organic Light Emitting Diode (OLED) is fixed on the rotatable substrate pedestal 10 in the high vacuum settling chamber 9 of cluster line gas-phase deposition system, the exiting surface of OLED is towards the line incident direction, then pedestal 10 is sealed in the high vacuum settling chamber 9, makes the exiting surface of LED be in the center of nanocluster line 8;
(b) air accumulation method cluster beam source 2 is connected on the vacuum chamber 7, air accumulation method cluster beam source 2 adopts the air accumulation method to produce the cluster line, utilize extract system mechanical pump, Lodz pump and molecular pump to vacuumize, the vacuum degree that makes high vacuum settling chamber 9 is 5 * 10
-5During Pa, charge into the argon gas 1 of 500Pa in the condensation chamber 5 of air accumulation method cluster beam source at inert gas entrance, under this air pressure, produce high density Ti atom gas by the atomizer 3 in the air accumulation method cluster beam source 2, Ti atom nucleating growth in argon gas forms the Ti cluster, by first order difference vacuum system 11 the Ti cluster in the condensation chamber 5 is ejected in the vacuum chamber 7 through nozzle 4 with argon gas, form Ti cluster line, making Ti cluster line by second level difference vacuum system 12 is that 2 millimeter first collimater 6 and second collimater 6 enter in the high vacuum settling chamber 9 through diameter, form the Ti nanometer particle beam 8 of high orientation, regulate input power, make Ti nanometer particle beam 8 deposition rates remain on about 1.2/s approximately;
(c) pedestal 10 in the rotation high vacuum settling chamber 9 makes the incidence angle of 8 one-tenth 0 ° of solid-state light emitters light output surface normal and Ti nanocluster line, controls Ti nanocluster line the OLED light output surface is deposited;
(d) deposition/oxidation hockets in Chen Ji the process, and every deposition 2min control beam flow baffle plate interception line stops deposition, then 9 feeding 50Pa, the 99.99% pure O to the high vacuum settling chamber
2Oxidation 30min takes out O after oxidation is finished
2Recover high vacuum and continue deposition, total time reach 30min until deposition through 6 deposition/oxidation cycle cycles, stop to deposit, obtain porous TiO as shown in Figure 2
2The how empty film of nano particle.TiO in the preparation of OLED die surfaces
2The nano particle porous membrane, the TiO of the present invention's preparation
2It is about 20% that the luminous efficiency of nanostructure OLED has improved, TiO
2The existence of nanoparticulate thin films does not produce any harmful effect to the electric property of OLED.
Claims (6)
1. one kind based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane, this method realizes that by nanocluster line depositing system its preparation methods steps is as follows:
(a) solid-state light emitters is fixed on the rotatable substrate pedestal (10) in the high vacuum settling chamber (9) of cluster line gas-phase deposition system, the exiting surface of luminous element is towards the line incident direction;
(b) air accumulation method cluster beam source (2) is connected on the vacuum chamber (7), air accumulation method cluster beam source (2) adopts the air accumulation method to produce particle beam, utilize the mechanical pump of extract system, lobe pump and molecular pump vacuumize cluster line depositing system, in condensation chamber (5), feed 50 ~ 500Pa inert gas (1), produce high density Ti atom by atomizer (3), Ti atom nucleating growth in inert gas (1) forms the Ti cluster, by first order difference vacuum system (11) the Ti cluster in the condensation chamber (5) is ejected in the vacuum chamber (7) through nozzle (4) with inert gas, form Ti cluster line, by second level difference vacuum system (12) Ti cluster line is entered in the high vacuum settling chamber (9) through first collimater (6) and second collimater (6), form the nanometer particle beam (8) of high orientation;
(c) pedestal (10) in the rotation high vacuum settling chamber (9), make solid-state light emitters light output surface normal direction become 0 °～85 ° angles with nanometer particle beam (8), utilize that oblique incidence deposition produces from masking effect, form the Ti nanoparticulate thin films of porous;
(d) in deposition process, feed the oxygen of 10 ~ 50Pa in high vacuum settling chamber (9), make the Ti nano particle be oxidized to TiO
2Nano particle, or the mode that adopts deposition/oxidation to hocket earlier at vacuum condition deposit one deck Ti nano particle, stop deposition then, and the aerating oxygen oxidation extracts oxygen after finishing oxidation, the continuation vacuum moulding machine, and the deposition/oxidation cycle by such makes TiO
2Nano particle reaches required coverage rate and the number of plies at the solid-state light emitters light output surface, stops deposition.
2. according to claim 1 a kind of based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane is characterized in that in the solid-state light emitters described in the step (a) it being the Organic Light Emitting Diode of GaN base, GaP light-emitting diode or emission visible light.
3. according to claim 1 a kind of based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane is characterized in that at the atomizer (3) described in the step (b) be to realize by magnetron sputtering or arc discharge.
4. according to claim 1 a kind of based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane, the size that it is characterized in that particle in nanometer particle beam (8) described in the step (b), control TiO by the air pressure that the distance between change atomizer (3) and the nozzle (4) or change charge into inert gas (1)
2The diameter of nano particle is 5 ~ 100nm.
5. according to claim 1 a kind of based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane is characterized in that regulating the porosity characteristic of nanoparticulate thin films depositing in oblique incidence described in the step (c) by the angle of oblique incidence deposition, regulates TiO thereby reach
2The purpose of particle film effective refractive index, the adjustable range of nanometer particle beam oblique incidence angle are 0 °～85 °.
6. according to claim 1 a kind of based on TiO
2The solid-state light emitters total internal reflection light outbound course of nano particle porous membrane is characterized in that preparing TiO described in the steps d
2The method of nano particle, in the mode that direct oxidation or deposition/oxidation hocket, the air pressure of aerating oxygen is 10 ~ 50Pa, oxidization time is 5min ~ 30min.
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| CN108332674A (en) * | 2018-02-11 | 2018-07-27 | 中国科学院电子学研究所 | The method that single spectrum seeks porous film thickness and porosity |
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| US20070298160A1 (en) * | 2006-06-22 | 2007-12-27 | Samsung Electronics Co., Ltd. | Thin film containing nanocrystal particles and method for preparing the same |
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