CN101582303A - Transparent conductive film with novel structure and preparation method thereof - Google Patents
Transparent conductive film with novel structure and preparation method thereof Download PDFInfo
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- CN101582303A CN101582303A CNA2009100801422A CN200910080142A CN101582303A CN 101582303 A CN101582303 A CN 101582303A CN A2009100801422 A CNA2009100801422 A CN A2009100801422A CN 200910080142 A CN200910080142 A CN 200910080142A CN 101582303 A CN101582303 A CN 101582303A
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Abstract
The invention discloses a transparent conductive film with novel structure and a preparation method thereof. The novel structure comprises a substrate 1, a buffer layer 1 and the transparent conductive film 3. The transparent conductive film 3 comprises a transparent conductive oxide material 4 and one or more high-conductivity one-dimensional conductive materials 5; wherein the one-dimensional conductive material is randomly distributed in the transparent conductive oxide. By combining the characteristics of the transparent conductive oxide and the one-dimensional conductive material, the electrical and optical properties of the transparent conductive film are improved. The invention also discloses a method for preparing the transparent conductive film of the novel structure.
Description
Technical field
The present invention relates to the solar cell field, transparent conductive film of especially a kind of new structure and preparation method thereof.
Background technology
Along with the development of photovoltaic power generation technology, a large amount of industrialization of thin film solar cell especially in recent years, there is very big technological challenge in transparent conductive oxide film (TCO) as necessary part in the thin film solar cell.Transparent conductive oxide (TCO) substrate as the thin film solar cell transparency electrode plays crucial effect for the conversion efficiency that improves battery.
Thin film solar cell requires transparency electrode to have extremely low light loss, high permeability and high conductivity.In recent years, the material of transparent conductive film is tending towards metal-oxide semiconductor (MOS), as SnO
2, In
2O
3With films such as ZnO, selected semi-conducting material, its energy gap width must be greater than visible light energy, could obtain high-penetrability at visible region, therefore energy gap requires greater than 3eV, but the conductivity of this pure semiconductor is still desirable not to the utmost, in order to increase its conductivity, usually can mix some impurity, a kind of be mix cation than former compound many monovalence metal ion or mix the nonmetallic ion that lacks monovalence than the anion of former compound; Second kind is to make the incomplete semiconducting compound of the state of oxidation, and forming in the semiconductor has anionic vacancy.But generally film transmitance and resistance are two factors of mutual contradiction, and when film thickness was thin, the transmitance of material was higher, but resistance is higher; When film thickness was thicker, the resistance of material was lower, but transmitance but can descend.This shows that it is most important coordinating the resistance of film and the performance of transmitance.
The one-dimensional electric material has obtained good development at present, and to 50 nanometers, length has had the one-dimensional material of many types can realize high-purity and high dispersive between 100 nanometers to 10 centimetre to diameter from 1 nanometer.In transparent conductive oxide film, mix a certain amount of one-dimensional electric material, can improve the electric conductivity of thin-film material, the thickness of film can reduce like this, be very beneficial for improving the transmitance of light, although the one-dimensional material itself that mixes is nontransparent, seeing through of meeting shading light, but as long as rationally reduce the doping content of film thickness and one-dimensional material, performance generally can improve the permeability of material light.
At present, the technology of preparation normal transparent conductive film has a lot, mainly comprise: magnetron sputtering technique, aumospheric pressure cvd (APCVD), low-pressure chemical vapor deposition (LPCVD), thermal evaporation deposition, sol-gelatin plating method, spray heating decomposition etc., wherein spray heating decomposition equipment is simple, not high to requirement for experiment condition such as vacuum, atmosphere, and reaction is easy to control; The range of choice of raw material is wide, and composition, forms and to be convenient to adjust.But, utilize the ullrasonic spraying thermal decomposition method on substrate, prepare this novel transparent conductive film that is mixed with the one-dimensional electric nano material also Shang Weiyou see.
The present invention is compound to the one-dimensional electric material in the transparent conductive film material, has proposed a kind of transparent conductive film of new structure, and has invented the method for preparing this new structure transparent conductive film with the ullrasonic spraying thermal decomposition method on substrate.
Summary of the invention
The present invention seeks in order to improve the electric conductivity of transparent conductive substrate, thereby improve the photoelectric conversion efficiency of thin film solar cell, finally invented a kind of structure of transparent conductive film, make its application that more can adapt to thin film solar cell, and invented the method for preparing this novel transparent conductive film in conjunction with the ripe ullrasonic spraying pyrolysis device and the manufacture craft of original preparation normal transparent conductive oxide film.
The present invention to achieve these goals, designed a kind of structure of transparent conductive film, this structure of transparent conductive film comprises substrate 1, resilient coating 2, transparent conductive film 3 three parts composition, is bottom with substrate 1, be followed successively by resilient coating 2, transparent conductive film 3 above, resilient coating 2 is mainly with SiO
2Be main, thickness in 10 nanometers between 100 nanometers, wherein resilient coating mainly plays the effect that strengthens stress between transparent conductive film and the substrate, stop Na ion and anti-reflection effect, in addition, in order to increase the electric conductivity of transparent conductive film, finally improve the photoelectric conversion efficiency of thin film solar cell, invented a kind of novel structure of transparent conductive film.In the transparent conductive oxide 4 of original comparative maturity, mix one-dimensional electric material 5, reduce the thickness of transparent conductive film by the high conduction performance of one-dimensional electric material, and then the transmitance of raising transparent conductive film, the doping content of one-dimensional electric material is 1wt%～0.01wt%, rationally adjust the doping content of film thickness and one-dimensional material, finally make this novel film material keep resistance to be equal to or less than under the normal transparent conductive film resistance situation, transmitance increases.
Transparent conductive film mainly comprises transparent conductive oxide material 4 and the high one-dimensional electric material 5 of conductivity among the present invention, wherein, transparent conductive oxide 4 mainly is selected from oxide and the composite multi-component oxide film material thereof of In, Sn, Zn and Cd, specifically can be: Sn doping In
2O
3Transparent conductive oxide, SnO
2In base transparent conductive oxide, zno-based transparent conductive oxide or CdO base transparent conductive oxide and other transparent conductive oxide one or more.
Described SnO
2The base nesa coating, its doped chemical comprises one or more of elements such as F, Sb, In, Zn, Mn, Sr, Zr, Ge, Ce, Pt, Pd, Cd, Nd.
Described zno-based nesa coating, its doped chemical comprises one or more in the elements such as F, Sb, Zr, Al, Ga.
Transparent conductive oxide 4 has that the forbidden band is wide, visible light and the high characteristic of near infrared spectrum district light transmission, and mean transmissivity is greater than 80%, and has certain electric conductivity, and resistivity is less than 10
-3Ω cm.
The main electric actions that rise of one-dimensional electric nano material 5, one-dimensional electric material 5 diameters are from 1nm to 50nm, and length is between 100 nanometers to 10 centimetre.
One-dimensional electric nano material 5 in the transparent conductive film 3 comprises: metal nanometer line, carbon nano-tube, in the materials such as metallic fiber or nano metal band one or more, the resistance of monodimension nanometer material 5, diameter and length can be carried out different selections according to material requirements and preparation technology's difference, the resistivity of one-dimensional electric material requires less than the transparent conductive oxide that is mixed, and reach minimum as far as possible, in addition, the diameter of one-dimensional electric material and length are keeping under the same resistivity condition, diameter and length are the smaller the better, to guarantee this one-dimensional electric nano material the film transmitance are caused very little influence.
The thermal decomposition method of ullrasonic spraying described in the present invention preparation process comprises the required precursor aqueous solution of preparation, and utilize supersonic oscillations that solution and one-dimensional electric nano material are fully mixed, the frequency of ultrasonic vibration is between 200kHz～1500kHz, and preferably clear conductive oxide and one-dimensional electric material are with the mixed of weight ratio 100/1～10000/1.Utilize current-carrying gas to drive then and make solution atomization, evaporation drying and cohesion, solution and one-dimensional electric nano material after promptly will atomizing with carrier gas are brought shower nozzle into, and carrier gas commonly used can be nitrogen, hydrogen or both mists etc.Carrying droplet and the one-dimensional electric nano material sprays equably through current-carrying gas behind the shower nozzle, enter reative cell, droplet solvent evaporates droplet in dropping process dwindles, fall graduation behind the underlay substrate surface of high temperature, unnecessary solvent gasification, remaining solid-state solute is subjected to the heating of substrate, temperature raises, thermal decomposition takes place in solute and steam reaction on substrate at last, and doped chemical also is incorporated in the film in reaction in the precursor aqueous solution, film forming on underlay substrate at last, meanwhile, the one-dimensional electric nano material is deposited to substrate surface with one of droplet, and being distributed in the transparent conductive material at random.The temperature of underlay substrate generally between 100 ℃～800 ℃, utilizes sedimentation time length to control the thickness of film, finally finishes the preparation of this novel transparent conductive film.
New structure transparent conductive film of the present invention can improve the optics and the electrology characteristic of transparent conductive film greatly, and utilizes this novel transparent conductive film of preparation of ullrasonic spraying thermal decomposition method success, and preparation technology is simple, is easy to control, is convenient to implement.
Description of drawings
Fig. 1 is the structure of transparent conductive film figure of new structure
Wherein, 1-substrate, 2-resilient coating, 3-transparent conductive film, 4-transparent conductive oxide, 5-one-dimensional electric nano material.
Embodiment
Below in conjunction with accompanying drawing technical solutions according to the invention are described in detail.
With reference to the accompanying drawings 1, this new structure transparent conductive film comprises that substrate-1, resilient coating-2, transparent conductive film-3 three part form, and is bottom with substrate-1, and the intermediate layer is a resilient coating-2.Wherein substrate is the float glass process ultra-clear glasses, and resilient coating is SiO
2, thickness is 50 nanometers, and transparent conductive film mainly comprises transparent conductive oxide material 4 and the high one-dimensional electric nano material 5 of conductivity, and wherein, transparent conductive oxide 4 is selected SnO for use
2: F, the transmitance of this TCO material is about 82%, and resistivity is 5 * 10
-4Ω cm; In order to increase the electric conductivity of transparent conductive film, the final photoelectric conversion efficiency that improves thin film solar cell, in the transparent conductive oxide 4 of original comparative maturity, mix one-dimensional electric material 5, reduce the thickness of TCO film by the high conduction performance of one-dimensional electric material, and then the transmitance of raising transparent conductive film, the doping content of one-dimensional electric nano material is 1wt%-0.01wt%, the one-dimensional electric nano material is selected conductive carbon nanotube for use among this embodiment, has the metallic conduction performance, doping content is 0.1wt%, transparent conductive film thickness is 500nm, and one-dimensional electric nano material 5 is randomly distributed in the transparent conductive oxide 4.
The preparation process for preparing above-mentioned novel transparent conductive film is as follows:
Present embodiment adopts general ullrasonic spraying thermal decomposer.
When preparing based on SnO
2: the used raw material of precursor aqueous solution during the novel transparent conductive film of F is SnCl
4, NH
4F and additive.The plated film solvent can be alcohol or water, alcohols preferred alcohol, butanols, and wherein the one-dimensional electric nano material is mixed with precursor aqueous solution; Depositing temperature is 100 ℃～800 ℃; Carrier gas flux is 0.1～10m
3/ h; Jet length is 0.1cm～100cm.
At first, configuration SnO
2: F precursor aqueous solution, wherein SnCl
4Solution concentration is 0.07g/ml; NH
4F:SnCl
4Quality is mixed than being 28%; The etoh solvent solution concentration is about 10%; The one-dimensional electric nano material is mixed in this precursor aqueous solution, and the concentration of mixing of one-dimensional electric nano material is 0.00006g/ml, and solution is evenly mixed, and the one-dimensional electric nano material is distributed in this precursor aqueous solution at random uniformly.
Regulate sprinkler height, underlay substrate is put into the reative cell of ullrasonic spraying thermal decomposer, the solution that configures is poured in the ultrasonic bottle, and opened heater, be warmed up to 450 ℃, and stable certain hour.
Open the carrier gas valve, began deposit film after ventilating about one minute, utilize sedimentation time length to control the thickness of film, deposited the back closing device, allow film lower the temperature naturally, finally finish the preparation of this novel transparent conductive film.
Claims (10)
1, a kind of transparent conductive film of new structure comprises substrate (1), resilient coating (2) and transparent conductive film (3), it is characterized in that, mixes one-dimensional electric material (5) in the transparent conductive oxide (4) of transparent conductive film (3).
2, transparent conductive film according to claim 1 is characterized in that, transparent conductive oxide (4) mean transmissivity is greater than 80%, and resistivity is less than 10
-3Ω cm.
3, transparent conductive film according to claim 1 and 2 is characterized in that, transparent conductive oxide (4) is selected from: Sn doping In
2O
3Transparent conductive oxide, SnO
2In base transparent conductive oxide, zno-based transparent conductive oxide or the CdO base transparent conductive oxide one or more.
4, transparent conductive film according to claim 3 is characterized in that, SnO
2The base nesa coating, doped chemical is one or more of F, Sb, In, Zn, Mn, Sr, Zr, Ge, Ce, Pt, Pd, Cd or Nd; Zno-based nesa coating, doped chemical are one or more among F, Sb, Zr, Al or the Ga.
According to described any one transparent conductive film of claim 1～4, it is characterized in that 5, the resistivity of one-dimensional electric material (5) is less than the transparent conductive oxide that is mixed, and reach minimum as far as possible.
According to described any one transparent conductive film of claim 1～5, it is characterized in that 6, one-dimensional electric material (5) is one or more of metal nanometer line, carbon nano-tube, metallic fiber or nano metal band; One-dimensional electric material (5) diameter be 1 nanometer to 50 nanometers, length is from 100 nanometers to 10 centimetre.
7, according to described any one transparent conductive film of claim 1～6, it is characterized in that one-dimensional electric material (5) being distributed in the transparent conductive oxide (4) at random; The doping content of one-dimensional electric material is 1wt%～0.01wt%.
8, according to the preparation method of described any one transparent conductive film of claim 1～7, it is characterized in that, utilize the ullrasonic spraying thermal decomposition method to go up the novel transparent conductive film that preparation is mixed with one-dimensional electric material (5) at substrate (1).
9. preparation method according to claim 8, it is characterized in that, comprise: prepare required precursor aqueous solution, and utilize supersonic oscillations that solution and one-dimensional electric material are fully mixed, in ultrasonic atomizer, make the precursor aqueous solution atomizing, solution and one-dimensional electric material after will atomizing with carrier gas are then brought shower nozzle into, carrying droplet and the one-dimensional electric material sprays equably through current-carrying gas behind the shower nozzle, enter reative cell, droplet solvent evaporates droplet in dropping process dwindles, and falls graduation behind the underlay substrate surface, meanwhile, the one-dimensional electric material is deposited to substrate surface with one of droplet, last pyrolysis, film forming on substrate.
10. according to Claim 8 or 9 described preparation methods, it is characterized in that depositing temperature is 100 ℃～800 ℃; Carrier gas flux is 0.1～10m
3/ h.
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|---|---|---|---|
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| CN101887920A (en) * | 2010-06-25 | 2010-11-17 | 蚌埠玻璃工业设计研究院 | Transparent conductive film glass of solar battery and production method thereof |
| CN102467272A (en) * | 2010-11-08 | 2012-05-23 | 智盛全球股份有限公司 | Transparent conductive structure with nano-scale conductive mixture and manufacturing method of transparent conductive structure |
| CN102971805A (en) * | 2010-02-27 | 2013-03-13 | 因努瓦动力有限公司 | Structures with surface-embedded additives and related manufacturing methods |
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