CN1442872A - Multilayer nano transparent conductive membrane and its preparation method - Google Patents
Multilayer nano transparent conductive membrane and its preparation method Download PDFInfo
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Abstract
A multilayered nano transparent conductive film is of alternate structures of dielectric layer and metal layer, and the metal layer is between two dielectric layers which are symmetric in structure or non-symmetric in structure. Its preparing method is to first work out a computer analog program for photoelectric performance of multilayer film according to the characteristic metrix calculation formula of multilayer, the theory of plasma resonance and the electronic transport in metal continuous film, to optimize the design of D/M/D multilayer film structure including selecting and matching of material quality, film thickness, reflecting rate and conductive rate, predicting of several kinds for D/M/D multilayer film structure, and then to use vacuum vaporation coating method to make D/M/D multilayer film by using accurate film thickness detection system to record film thickness
Description
Technical field
What the present invention relates to is a kind of nanometer transparent conducting film and preparation method thereof, and multi-layer nano nesa coating of particularly a kind of not only transparent but also conduction that is used for the flat-panel screens transparency electrode and preparation method thereof belongs to the nano film material field.
Background technology
Transparent conductive film not only should have good electric conductivity, also should have fine visible light transmissivity and to the infrared waves reflecting properties.Mix Sn indium oxide film (ITO) owing to have at visible region high transmission rate (~ 85%) with than low resistance, but also has good etching, therefore, often be widely used in flat liquid crystal display (LCD), electroluminescence and show the electrode film of (ELD), Plasma Display (PD), solar cell and energy-conservation infrared reflection film etc.Dielectric/metal/dielectric (D/M/D) multilayer film has been used as a kind of important low emissivity film (heat mirror) and has been used widely the eighties in last century.But it is few that it works as fashion as the research report of transparent conductive film.Find by literature search, people such as M.Bender in 1998 and W.Seelig write articles " Dependence of film composition andthicknesses on optical and electrical properties of ITO-metal-ITOmultilayers (relation of ITO-metal-ITO multilayer film photoelectric properties and its thickness and composition) " on " ThinSolid Films " the 326th (1998) 67-71, this article proposes to replace single ito thin film with ITO/Ag/ITO (I/M/I) multilayer film, figures for better electric conductivity and lower cost.But, the ITO film is as deielectric-coating, its refractive index (n ~ 2.0) and resistivity (than high 2～3 orders of magnitude of Ag, Cu) are also not really desirable, it subdues reflex and leakage current is not good enough, the I/M/I photoelectric properties of sandwich structure do not reach people's desired value as yet, 50nmITO/12nm AgCu/50nmITO electric property is the highest in 5 kinds of structures introducing in this article, and its value only is 24.6 * 10
-3Ω
-1In addition single relatively ITO film is in I/M/I, although the ITO consumption reduces to some extent, the preparation technology of I/M/I adopts dc magnetron reactive sputtering, control the voltage ratio of reasonable oxygen, argon gas, technology is rather complicated, also need heat reprocessing sometimes, so production cost is still very high.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of D/M/D multi-layer nano nesa coating and preparation method thereof is provided, make its superior performance, with low cost.The present invention is achieved by the following technical solutions, dielectric/metal/dielectric of the present invention (D/M/D) multi-layer nano nesa coating is dielectric and metal level alternating structure, is metal level in the middle of the two-layer dielectric, wherein dielectric layer can be a symmetrical structure, also can be unsymmetric structure.
Its intermediate layer is an argent, and its thickness is 12～18nm, and composite diffusion barrier layer improves thermal stability, dielectric layer thickness 40～166nm.The D/M/D symmetrical structure of multi-layer nano nesa coating, promptly the dielectric substance of metal level both sides is identical, and thickness equates; D/M/D structure unsymmetric structure has two kinds of situations, and a kind of is the material difference, and thickness is identical, and a kind of is thickness same material difference.Unsymmetric structure (D
1/ M/D
2) middle material difference, when thickness was identical, it be n that its refractive index is selected
1∠ n
2
Because metals such as Ag, Cu have the best electrical conductivity energy, its conductivity is than high about two orders of magnitude of ITO film; ZnS, TiO
2The height of refractive index ratio ITO film, its n value is respectively 2.3 and 2.2, they can make light equate and anti-phase in dielectric layer front and rear surfaces reverberation amplitude as deielectric-coating and when selecting appropriate thickness, interfere mutually and offset, and play good anti-reflection effect.In addition, ZnS, TiO
2All be dielectric material, its resistivity is more than ITO film height, so leakage current is little, therefore the D/M/D multi-layer nano-film of a fixed structure can have than ITO or the better photoelectric properties of I/M/I, can be used as the usefulness of the transparency electrode of flat-panel screens.Here the thickness of metal film affects the photoelectric properties of D/M/D multilayer film significantly.Metal is lepthymenia, can not form continuous film this moment and is island and distributes, because island structure worsens its electric conductivity to the scattering and the boundary effect of electron waves, its square resistance rises rapidly; Blocked up, though help reducing its square resistance, its light transmission sharply descends, and promptly its light transmission and electric conductivity are a pair of contradiction, have the thickness of a best metal film.In addition, the all-in resistance of D/M/D multilayer film (square resistance) comes from three independently rete D
1, D
2With the resistance of M, according to the resistance parallel model, can be according to total square resistance of the resistance calculations D/M/D of each rete:
Because the resistance of deielectric-coating is higher than the resistance of metal film, R widely
D" R
M, so the square resistance of D/M/D depends primarily on the resistance of metal film.Therefore the accurate control of the selection of metal film and thickness is that the D/M/D multilayer film is obtained one of key of good photoelectric properties; Simultaneously, each layer material, thickness ratio and interlayer structure all influence final photoelectric properties among the D/M/D.Be the influence of refractive index equally to light transmission, the refractive index n of upper layer film
1Refractive index n with underlying membrane
2Influence degree be different; Owing to can produce diffusion and interfacial reaction in system film and the stabilization processes process subsequently, the existence of interfacial reaction product not only influences the photoelectric properties index, and can influence uniformity of color or the like between each rete of D/M/D.
The preparation method of multi-layer nano nesa coating of the present invention, at first according to the eigenmatrix computing formula of multilayer film, electron transport and the plasma resonance theory in (metal) continuous film, the computer simulator of establishment multilayer film photoelectric properties, optimal design D/M/D multi-layer film structure, this comprises the selection of material, thickness, refractive index, conductivity and coupling etc., and prediction has some kinds of D/M/D multi-layer film structures of optimal light electrical property; Method with vacuum evaporation prepares the D/M/D multilayer film then, the admittance matching process that replaces optical monitoring prepares the ITO/Ag/ITO film, simultaneously when evaporation, except that coming the dynamically recording thickness with accurate film thickness monitoring system, also not timing sampling and measuring thickness is also proofreaied and correct, it is accurately errorless to make every effort to thickness, to obtain spectral performance in a big way, makes the D/M/D multilayer film have better selection optical filtering performance and color balance.
Method with vacuum evaporation prepares the D/M/D multilayer film, system's base vacuum 1.0 * 10
-2～8.5 * 10
-2Pa behind ion beam bombardment substrate 10～15min, is evacuated to 5.0 * 10 with vacuum again
-3～8.5 * 10
-3Pa, deposition rate is 0.2～0.5nm/s, base reservoir temperature is about 25～45 ℃.Thickness is monitored in real time by quartz oscillation film thickness monitoring instrument in the film preparation process, and accurately measures its thickness with ellipsometer test or with X-ray electricity spectrum (XPS).
Mate for the material of improving or avoid inter-level diffusion and interfacial reaction problem, the present invention to carry out between deielectric-coating and the metal film, between deielectric-coating and metal film, increase diffusion barrier or cache layer, thereby develop into four layers or five tunic systems.
Since in the D/M/D multilayer film with upper layer film D
1What contacted is air, and with underlying membrane D
2What contact is base material (quartz glass), so D
1And D
2Layer is different to the influence of multilayer film optical property.Along with D
1The increase of tunic thickness, transmission peaks peak value descend gradually and move to the long wave direction, and the logical wave band of filter narrows down a little, and reflection paddy rises gradually and moves to the long wave direction, however D
1The tunic varied in thickness does not influence the absorption spectra of multilayer film; Along with D
2The increase of tunic thickness, the max transmissive peak change is little and peak position moves to the long wave direction, and new transmission peaks can appear in multilayer film transmission spectrum shortwave district, and the absorption spectrum of multilayer film is not subjected to D
2The influence of layer thickness variation.As for the influence of the refractive index of deielectric-coating, then be with D
1Layer refractive index n
1Increase, the transmission peaks of D/M/D multilayer film and reflection peak have small reduction, and move to the long wave direction, but along with D
2Layer refractive index n
2Increase, the transmission peaks of D/M/D multilayer film raises gradually, the logical waveband width of filter becomes big, transmission peaks and reflection paddy do not move horizontally.While D
2The surface roughness affect of layer the roughness and the interface definition of whole system rete, and D
1Layer only influences itself.Therefore, the present invention is different with the design philosophy of conventional I TO/M/ITO multilayer film, and it had both comprised symmetrical structure (D
1=D
2), also comprise unsymmetric structure (D
1≠ D
2), and in unsymmetric structure, comprise two kinds of situations, the one, D
1With D
2Identical and their the thickness differences of material, the 2nd, D
1With D
2Material is also different.According to the Film Optics theory, when optics thickness of film increased λ/2 (vertical incidence), the reflectivity of film was constant at λ wavelength place, also is that transmissivity is constant at this wavelength place.Therefore, unsymmetric structure D/M/D multilayer film can obtain good photoelectric properties equally.
The present invention has substantive distinguishing features and marked improvement, and the present invention has adopted the computer aided optimum design to replace the optical monitoring that admittance is mated, and adopts ZnS, the TiO of nontoxic cheapness
2Make raw material in dielectric and argent, vacuum evaporation, with low cost, can obtain high conductivity R
s=3.0 Ω/, high transmission of visible light T (550nm)=90%, high infrared reflectivity R
2500＞95%; The electric property F of optimum structure
TC＞100 * 10
-3Ω
-1These indexs are all considerably beyond ITO and I/M/I film.
Embodiment
Provide following examples to come the present invention is done further statement in conjunction with content of the present invention:
Embodiment 1:40nmTiO
2/ 18nmAg/40nmTiO
2
By the computer optimization structure Ag film is divided into 12nm, 15nm, three series of 18nm, to TiO
2Be the structure of dielectric layer, TiO
2Thickness do full search in 10～200nm scope, and with T
1 μ mAnd R
1700The symmetrical optimum structure that obtains as evaluation index is: 40nm TiO
2/ 18nmAg/40nm TiO
2Its preparation process is as follows: substrate: quartz crystal polishing section 35nm * 20nm * 1nm and Si (111) sheet.Adopt chemistry and ultrasonic waves for cleaning.Base reservoir temperature is 45 ℃.Vacuum degree: background vacuum 1 * 10
-2Pa behind ion beam bombardment substrate 15min, is evacuated to 1 * 10 with vacuum again
-3Pa.Raw material and heating source: Ag:99.9% particle, the heating of molybdenum boat resistance wire; TiO
2: 99.9% particle, the heating of tantalum boat electron gun.Deposition rate is 0.3nm/s.THICKNESS CONTROL: thickness is monitored in real time by quartz oscillation film thickness monitoring instrument in the film preparation process, and accurately measures its thickness with ellipsometer test.
The photoelectric properties index of this multi-layer nano-film:
| Thin-film material and each layer thickness | Square resistance Ω/ | Transmissivity % 550nm | Reflectivity % 2500nm | ????F TC(10 -3Ω -1) |
| 40nmTiO 2/18nmAg/40nmTiO 2 | ???3.0 | ??89.3 | ??＞95 | ????107 |
Embodiment 2:40nmZnS/18nmAg/40nmZnS
Substrate: Si (111) face, the SiO of the autoxidation of the about 5.0nm in surface
2Layer; Base reservoir temperature: 25 ℃, clean: general chemistry is cleaned back ultrasonic waves for cleaning 10min.System's base vacuum: 1 * 10
-3Pa.Deposition rate is 0.4nm/s.THICKNESS CONTROL: thickness is monitored in real time by quartz oscillation film thickness monitoring instrument in the film preparation process, and accurately measures its thickness with ellipsometer test.
The photoelectric properties index of this multi-layer nano-film:
| Thin-film material and each layer thickness | Square resistance Ω/ | Transmissivity % 550nm | Reflectivity % 2500nm | ???F TC(10 -3Ω -1) |
| 40nmZnS/18nmAg/40nmZnS | ??3.0 | ??＞90 | ??＞95 | ???116 |
Embodiment 3:40nmTiO
2/ 18nmAg/166nmTiO
2
Substrate: quartz crystal polishing section 35nm * 20nm * 1nm and Si (111) sheet.Adopt chemistry and ultrasonic waves for cleaning.Base reservoir temperature is 45 ℃.Vacuum degree: background vacuum 3.5 * 10
-2Pa behind ion beam bombardment substrate 12min, is evacuated to 3.0 * 10 with vacuum again
-3Pa.Raw material and heating source: Ag:99.9% particle, the heating of molybdenum boat resistance wire; TiO
2: 99.9% particle, the heating of tantalum boat electron gun.Deposition rate is 0.3nm/s.THICKNESS CONTROL: thickness is monitored in real time by quartz oscillation film thickness monitoring instrument in the film preparation process, and accurately measures its thickness with ellipsometer test.
The photoelectric properties index of this multi-layer nano-film:
| Thin-film material and each layer thickness | Square resistance Ω/ | Transmissivity % 550nm | Reflectivity % 2500nm | ????F TC??(10 -3Ω -1) |
| 40nmTiO 2/18nmAg/166nmTiO 2 | ??3.0 | ????80 | ????＞90 | ????35.8 |
Embodiment 4:40nmTiO
2/ 12nmAg/40nmTiO
2
Substrate: Si (111) sheet.Adopt chemistry and ultrasonic waves for cleaning.Base reservoir temperature is 45 ℃.Vacuum degree: background vacuum 3.5 * 10
-2Pa behind ion beam bombardment substrate 15min, is evacuated to 4.5 * 10 with vacuum again
-3Pa.Raw material and heating source: Ag:99.9% particle, the heating of molybdenum boat resistance wire; TiO
2: 99.9% particle, the heating of tantalum boat electron gun.Deposition rate is 0.3nm/s.THICKNESS CONTROL: thickness is monitored in real time by quartz oscillation film thickness monitoring instrument in the film preparation process, and accurately measures its thickness with ellipsometer test.
The photoelectric properties index of this multi-layer nano-film:
| Thin-film material and each layer thickness | Square resistance Ω/ | Transmissivity % 550nm | Reflectivity % 2500nm | ????F TC??(10 -3Ω -1) |
| 40nmTiO 2/12nmAg/40nmTiO 2 | ???8.5 | ??91.5 | ??＞90 | ????48.4 |
Claims (8)
1, a kind of multi-layer nano nesa coating is characterized in that, is metal level in the middle of the two-layer dielectric, and wherein dielectric layer is a symmetrical structure, perhaps unsymmetric structure.
2, multi-layer nano nesa coating according to claim 1 is characterized in that, its intermediate layer is an argent, and its thickness is 12～18nm, improves thermal stability, dielectric layer thickness 40～166nm by composite diffusion barrier layer.
3, multi-layer nano nesa coating according to claim 1 is characterized in that, the dielectric/metal of multi-layer nano nesa coating/dielectric symmetrical structure, and promptly the dielectric substance of metal level both sides is identical, and thickness equates; Dielectric/metal/dielectric unsymmetric structure has two kinds of situations, and a kind of is the material difference, and thickness is identical, and a kind of is that thickness is identical, the material difference.
4, multi-layer nano nesa coating according to claim 3 is characterized in that, in dielectric/metal/dielectric unsymmetric structure, when the material different-thickness was identical, its refractive index was upper layer film n
1∠ underlying membrane n
2
5, a kind of preparation method of multi-layer nano nesa coating, it is characterized in that, at first according to the eigenmatrix computing formula of multilayer film, electron transport and plasma resonance theory in the metal continuous film, the computer simulator of establishment multilayer film photoelectric properties, optimal design D/M/D multi-layer film structure, this comprises the selection of material, thickness, refractive index, conductivity and coupling etc., predicts some kinds of D/M/D multi-layer film structures; Method with vacuum evaporation prepares the D/M/D multilayer film then, simultaneously when evaporation, comes the dynamically recording thickness with accurate film thickness monitoring system, and the sampling and measuring thickness is also proofreaied and correct at any time.
6, the preparation method of multi-layer nano nesa coating according to claim 5 is characterized in that, prepares the D/M/D multilayer film, system's base vacuum 1.0 * 10 with the method for vacuum evaporation
-2～8.5 * 10
-2Pa behind ion beam bombardment substrate 10～15min, is evacuated to 5.0 * 10 with vacuum again
-3～8.5 * 10
-3Pa, deposition rate is 0.2～0.5nm/s, base reservoir temperature is 25～45 ℃.
7, the preparation method of multi-layer nano nesa coating according to claim 5 is characterized in that, thickness is monitored in real time by quartz oscillation film thickness monitoring instrument in the film preparation process, and accurately measures its thickness with ellipsometer test or with X-ray electricity spectrum.
8, the preparation method of multi-layer nano nesa coating according to claim 5, it is characterized in that, improve or avoid inter-level diffusion and interfacial reaction to adopt following method: carry out the material coupling between deielectric-coating and the metal film, between deielectric-coating and metal film, increase diffusion barrier or cache layer, develop into four layers or five tunic systems.
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| CN100462749C (en) * | 2006-08-31 | 2009-02-18 | 甘国工 | Filter plate having electromagnetic radiation prevention and light filtering function of plasma display |
| CN101441325B (en) * | 2007-11-20 | 2010-08-11 | 中国科学院光电技术研究所 | Design method of multilayer metal dielectric film capable of realizing imaging function |
| CN102683240A (en) * | 2012-05-09 | 2012-09-19 | 上海宏力半导体制造有限公司 | Method for evaluating performance of deposited film |
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| CN103777417B (en) * | 2007-04-20 | 2017-01-18 | 凯姆控股有限公司 | Composite transparent conductors and methods of forming the same |
| CN103777417A (en) * | 2007-04-20 | 2014-05-07 | 凯博瑞奥斯技术公司 | Composite transparent conductors and methods of forming the same |
| CN101441325B (en) * | 2007-11-20 | 2010-08-11 | 中国科学院光电技术研究所 | Design method of multilayer metal dielectric film capable of realizing imaging function |
| CN104752626A (en) * | 2008-03-13 | 2015-07-01 | 应用材料公司 | Water-barrier encapsulation method |
| CN102683240A (en) * | 2012-05-09 | 2012-09-19 | 上海宏力半导体制造有限公司 | Method for evaluating performance of deposited film |
| CN102683240B (en) * | 2012-05-09 | 2017-06-09 | 上海华虹宏力半导体制造有限公司 | The method that assessment deposit forms film performance |
| CN104781935A (en) * | 2012-10-30 | 2015-07-15 | 皮尔金顿集团有限公司 | Silver based transparent electrode |
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| CN105700735B (en) * | 2014-12-09 | 2018-10-09 | Tdk株式会社 | Transparent conductive body and touch screen |
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| CN104835716A (en) * | 2015-03-18 | 2015-08-12 | 浙江大学 | Transparent conductive oxide film based on Ir interlayer doping |
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| CN105845028A (en) * | 2016-05-19 | 2016-08-10 | 信利（惠州）智能显示有限公司 | Application of transparent conductive film and silver nanowires in display |
| CN109036849A (en) * | 2018-06-29 | 2018-12-18 | 南京理工大学 | Voltage-controlled varactor of inorganic flexible all-transparent perovskite oxide and preparation method thereof |
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| CN112180648A (en) * | 2019-07-03 | 2021-01-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Optical film structure, preparation method and application thereof |
| CN112180648B (en) * | 2019-07-03 | 2022-04-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Optical film structure, preparation method and application thereof |
| CN112951930A (en) * | 2021-01-29 | 2021-06-11 | 山东省科学院能源研究所 | Titanium dioxide/silver/titanium dioxide transparent conductive film and preparation method and application thereof |
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