CN104561941A - Method for preparing NZO transparent conductive film - Google Patents
Method for preparing NZO transparent conductive film Download PDFInfo
- Publication number
- CN104561941A CN104561941A CN201510032546.XA CN201510032546A CN104561941A CN 104561941 A CN104561941 A CN 104561941A CN 201510032546 A CN201510032546 A CN 201510032546A CN 104561941 A CN104561941 A CN 104561941A
- Authority
- CN
- China
- Prior art keywords
- nzo
- transparent conductive
- conductive film
- colloidal sol
- sodium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
Abstract
The invention relates to the technical field of semiconductor manufacturing and in particular relates to a method for preparing an NZO transparent conductive film. The method comprises the following steps: adopting sodium bicarbonate to replace the traditional sodium carbonate so as to serve as a doping agent, forming multiple types of sol of different sodium/zinc ion ratios in the preparation of the NZO transparent conductive film, sequentially coating, rotating and annealing, and forming a functionally gradient film. The light transmission, conductivity and stability of the NZO transparent conductive film with the functional gradient are greatly improved.
Description
Technical field
The present invention relates to technical field of manufacturing semiconductors, particularly relate to a kind of method preparing NZO transparent conductive film.
Background technology
NZO (Na doping ZnO transparent conductive film), as a kind of good semiconductor material, can be applicable to window material and the field such as antireflection layer thin-film material and gas sensor of solar cell, and becomes ITO (In gradually
2o
3: Sn) etc. the potential replacer of transparent conductive film, its lower infrared emittance and higher infrared reflectance make it be used widely in adiabatic transparent material.
The method being prepared NZO transparent conductive film in existing technology of preparing includes: magnetron sputtering method (physical vapor deposition (Physical Vapor Deposition, PVD) one), SOL-GEL (sol-gel processing, prepare the brand-new method of one in the wet chemical method of material) method, pulsed laser deposition (Pulsed Laser Deposition, be called for short PLD, laser is utilized to bombard object, then by bombardment species precipitate out on different substrates, be precipitated or a kind of means of film) and CVD sedimentation.
Wherein, traditional SOL-GEL method has that cost is low, technique simply, easily realizes multi-element doping and can accurately control the various features such as film doping concentration.
In the process of this SOL-GEL legal system for NZO transparent conductive film, the raw material of Na doped source is Na
2cO
3and carrying out in spin coating proceeding step, adopting the film of single tunic or multilayer same concentrations to adulterate successively; Na
2cO
3material not easily realizes the Uniform Doped of Na, and adopt traditional spin coating proceeding only can obtain the NZO transparent conductive film of single concentration, greatly reduce the performance of NZO transparent conductive film, also there is technique instability in this SOL-GEL method simultaneously, the NZO transparent conductive film second-rate (as light transmission and conductivity etc.) of preparation, repeatable poor, be difficult to realize many defects such as suitability for industrialized production, these are all that those skilled in the art undesirably see.
Therefore, need badly and provide a kind of novel SOL-GEL legal system for NZO transparent conductive film, make it overcome above-mentioned defect, day by day become the direction that those skilled in the art are devoted to study.
Summary of the invention
In view of the above problems, the invention provides a kind of method based on SOL-GEL and prepare NZO transparent conductive film, the defect that traditional way prepares NZO transparent conductive film can be overcome to a great extent, to realize the light transmission, electroconductibility, the stability that improve NZO transparent conductive film by the method.
The present invention solves the problems of the technologies described above adopted technical scheme:
Prepare a method for NZO transparent conductive film, wherein, described method comprises:
Step S1, a certain amount of two acetate hydrate zinc solutions are dissolved in ethylene glycol monomethyl ether solvent, sodium hydrogen carbonate solution is added again afterwards in ethylene glycol monomethyl ether solvent, and the stablizer equal with zinc component molar ratio in described two acetate hydrate zinc solutions, to form some parts, there is identical zinc ion concentration, and sodium/zine ion is than different sample solutions;
Step S2, each described sample solution is carried out magnetic agitation, to form the colloidal sol corresponding to each described sample solution;
Step S3, the colloidal sol of the sample solution with minimum sodium/zine ion ratio is evenly coated on the silicon substrate of a rotation, carries out anneal, to form one deck NZO transparent conductive film in this silicon substrate upper surface;
Step S4, on the described NZO transparent conductive film of previously preparation, evenly coating one deck colloidal sol rotates, and carries out anneal, to continue to form another layer of NZO transparent conductive film in the described NZO transparent conductive film upper surface of previously preparation;
Repeat step S4, wherein, the sodium/zine ion of the colloidal sol applied each time is than the sodium/zine ion ratio being all greater than previous primary coating colloidal sol.
Preferably, above-mentioned method, wherein, described stablizer is monoethanolamine solvent.
Preferably, above-mentioned method, wherein, described step S2 comprises:
Each described sample solution is carried out magnetic agitation 3h respectively under the constant temperature of 85 DEG C, to form colloidal sol corresponding to each described sample solution.
Preferably, above-mentioned method, wherein, after forming colloidal sol corresponding to each described sample solution, also comprises and carries out still aging process to each described colloidal sol.
Preferably, above-mentioned method, wherein, the time of described still aging process is 48h.
Preferably, above-mentioned method, wherein, in described some sample solutions, sodium/zine ion ratio is respectively 1.5at%, 2.5at%, 4.0at%, 6.0at%, 8.0at%.
Preferably, above-mentioned method, wherein, step S3 specifically comprises:
The colloidal sol of the described sample solution of minimum sodium/zine ion ratio is evenly coated on the silicon substrate that rotating speed is 4000r/min and carries out rotation 30s, and 10min anneal under 350 DEG C of conditions is carried out to this colloidal sol.
Preferably, above-mentioned method, wherein, described two acetate hydrate zinc solutions, described ethylene glycol monomethyl ether solvent, described stablizer and described sodium hydrogen carbonate solution are analytical pure.
Technique scheme tool has the following advantages and beneficial effect:
The invention discloses a kind of method preparing NZO transparent conductive film, traditional sodium carbonate is replaced to be doping agent by adopting sodium bicarbonate, and carrying out in the preparation of NZO transparent conductive film, carry out successively applying by the colloidal sol forming multiple different sodium/zine ion ratio, rotate, anneal, to form function gradient film, greatly enhance light transmission, electroconductibility, the stability of the NZO transparent conductive film with functionally gradient.
Concrete accompanying drawing explanation
By reading the detailed description done non-limiting example with reference to the following drawings, the present invention and feature, profile and advantage will become more apparent.Mark identical in whole accompanying drawing indicates identical part.Proportionally can not draw accompanying drawing, focus on purport of the present invention is shown.
Fig. 1 is the method flow schematic diagram preparing NZO transparent conductive film in the present invention;
Fig. 2 is the structural representation of the NZO transparent conductive film in the present invention with functionally gradient.
Embodiment
Core concept of the present invention is: the preparation carrying out NZO transparent conductive film by changing the selection of colloidal sol raw material and proportioning and spin-coating technique, to improve light transmission, electroconductibility, the stability of NZO transparent conductive film.
Below in conjunction with accompanying drawing and specific embodiment, the present invention is further illustrated, but not as limiting to the invention.
For NZO transparent conductive film second-rate (as light transmission and conductivity etc.) prepared by traditional way, repeatable poor, being difficult to realize many defects such as suitability for industrialized production, the invention provides a kind of by utilizing the method for SOL-GEL to prepare NZO transparent conductive film.
This SOL-GEL legal system relates to the concept of a kind of Functionally Graded Materials FGM for NZO transparent conductive film, FGM refers to that component, properity etc. are with space or Time Continuous change or the high performance material of graded, it with the fundamental difference of conventional composite materials be exactly the consecutive variations of its microstructure, consecutive variations on composition can cause the graded of performance or structure.Under the enlightenment of Functionally Graded Materials, derive the concept of function gradient film.Function gradient film material makes composition exactly, organizes from matrix to surface is without interface consecutive variations.Function gradient film is due to the structure of its uniqueness, the composition of film and tissue is made to be transition state, can relief of thermal stress and internal stress greatly, thus make the structure organization performance of thin-film material more stable, and improve the bonding force of film and substrate, the film of grade doping also plays obvious effect alleviating on lattice mismatch between layers.Therefore based on this concept, SOL-GEL legal system is utilized to get everything ready the NZO transparent conductive film of functionally gradient, as shown in Figure 1 concrete.
Just the invention provides a specific embodiment to be below further elaborated.
First, the quantitative molten Zn (CH of two acetate hydrate zinc solutions is provided
3cOO)
2.
2h
2o as presoma, ethylene glycol monomethyl ether as solvent, monoethanolamine as stablizer, sodium bicarbonate NaHCO
3for doped solution, carry out following steps afterwards:
Step S1, by a certain amount of Zn (CH
3cOO)
2.
2h
2o solution is dissolved in ethylene glycol monomethyl ether solvent, adds NaHCO more afterwards in ethylene glycol monomethyl ether solvent
3solution, and with Zn (CH
3cOO)
2.
2h
2the stablizer (i.e. monoethanolamine solvent) that in O solution, Zn component molar ratio is equal, the sample solution of 1.5at%, 2.5at%, 4.0at%, 6.0at%, 8.0at% is respectively to form Zn ionic concn for 1.20mol/L, Na ion/Zn ion ratio.
Wherein, above-mentioned Zn (CH
3cOO)
2.
2h
2o solution, ethylene glycol monomethyl ether solvent, stablizer and NaHCO
3solution is analytical pure.Certainly, those skilled in the art can carry out other proportionings selection of above-mentioned Na ion/Zn ion ratio according to concrete process requirements, and the sample solution of some other quantity, but on the present invention all without substantial impact.
Step S2, the sample solution being 1.5at%, 2.5at%, 4.0at%, 6.0at%, 8.0at% by the Na ion/Zn ion ratio obtained in step S2 carry out magnetic agitation, respectively at a constant temperature to form colloidal sol corresponding to each sample solution; Wherein, in each colloidal sol, Na ion/Zn ion ratio is also 1.5at%, 2.5at%, 4.0at%, 6.0at%, 8.0at%.
Preferably, in an embodiment of the present invention, the sample solution of 1.5at%, 2.5at%, 4.0at%, 6.0at%, 8.0at% is carried out magnetic agitation 3h respectively under the constant temperature of 85 DEG C, to form colloidal sol corresponding to each sample solution.
Afterwards, still aging process is carried out after 48 hours to the colloidal sol that above-mentioned each sample solution correspondence is formed, carries out follow-up spin-coating.
Step S3, carry out spin-coating technique, first will there is the colloidal sol of the sample solution of minimum sodium/zine ion ratio, the silicon substrate (substrate of monocrystalline substrate, other materials or glass on) that the colloidal sol formed by Na ion/Zn ion ratio sample solution that is 1.5at% is evenly coated in rotation rotates, and anneal is carried out to this colloidal sol, to form one deck NZO transparent conductive film at the upper surface of this silicon substrate.
Preferably, this step can be specially: be that colloidal sol that the sample solution of 1.5at% is formed evenly is coated on silicon substrate that rotating speed is 4000r/min and carries out rotation 30s by Na ion/Zn ion ratio, afterwards, 10min anneal under 350 DEG C of conditions is carried out, to form one deck NZO transparent conductive film to this colloidal sol.
Step S4, on the NZO transparent conductive film of above-mentioned preparation, evenly other colloidal sol of coating one deck rotates, and carries out anneal, finally continues to form another layer of NZO transparent conductive film at the NZO transparent conductive film upper surface of above-mentioned preparation.Continue to repeat this step S4, and in this process, the sodium/zine ion of the colloidal sol applied each time is than the sodium/zine ion ratio being all greater than previous primary coating colloidal sol.
Concrete, after forming one deck NZO transparent conductive film (1.5at%) in step s3, be that the colloidal sol that the sample solution of 2.5at% is formed evenly is coated on this NZO transparent conductive film (1.5at%) and rotates by Na ion/Zn ion ratio, and anneal is carried out to this colloidal sol, to form another layer of NZO transparent conductive film (2.5at%) at this NZO transparent conductive film (1.5at%) upper surface.
Equally, for the colloidal sol that sodium/zine ion is formed than the sample solution for 4.0at%, 6.0at%, 8.0at%, all according to above-mentioned steps S4 process, the five layers of NZO transparent conductive film be positioned on silicon substrate are finally formed, as shown in Figure 2.
Wherein, in NZO transparent conductive film on this silicon substrate and by order on lower, Na ion/Zn ion ratio is followed successively by 1.5at%, 2.5at%, 4.0at%, 6.0at%, 8.0at%, and then common formation has the NZO structure of transparent conductive film of functionally gradient.This NZO transparent conductive film is prepared relative to traditional technology, no matter is all have great raising in light transmission, electroconductibility or stability.
Certainly, the number of plies of above-mentioned NZO transparent conductive film is only a preferably embodiment, those skilled in the art according to concrete process environments and can require the preparation carrying out the NZO transparent conductive film of the multiple number of plies, not merely be limited to above-mentioned five layers, even and if make variation and modify, on the present invention all without substantial impact.
In sum, the invention discloses a kind of method preparing NZO transparent conductive film, traditional sodium carbonate is replaced to be doping agent by adopting sodium bicarbonate, and carrying out in the preparation of NZO transparent conductive film, carry out successively applying by the colloidal sol forming multiple different sodium/zine ion ratio, rotate, anneal, to form function gradient film, greatly enhance light transmission, electroconductibility, the stability of the NZO transparent conductive film with functionally gradient.
It should be appreciated by those skilled in the art that those skilled in the art are realizing described change case in conjunction with prior art and above-described embodiment, do not repeat at this.Such change case does not affect flesh and blood of the present invention, does not repeat them here.
Above preferred embodiment of the present invention is described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, the equipment wherein do not described in detail to the greatest extent and structure are construed as to be implemented with the usual manner in this area; Any those of ordinary skill in the art, do not departing under technical solution of the present invention ambit, the Method and Technology content of above-mentioned announcement all can be utilized to make many possible variations and modification to technical solution of the present invention, or being revised as the Equivalent embodiments of equivalent variations, this does not affect flesh and blood of the present invention.Therefore, every content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent variations and modification, all still belongs in the scope of technical solution of the present invention protection.
Claims (8)
1. prepare a method for NZO transparent conductive film, it is characterized in that, described method comprises:
Step S1, a certain amount of two acetate hydrate zinc solutions are dissolved in ethylene glycol monomethyl ether solvent, sodium hydrogen carbonate solution is added again afterwards in ethylene glycol monomethyl ether solvent, and the stablizer equal with zinc component molar ratio in described two acetate hydrate zinc solutions, to form some parts, there is identical zinc ion concentration, and sodium/zine ion is than different sample solutions;
Step S2, each described sample solution is carried out magnetic agitation, to form the colloidal sol corresponding to each described sample solution;
Step S3, the colloidal sol of the sample solution with minimum sodium/zine ion ratio is evenly coated on the silicon substrate of a rotation, carries out anneal, to form one deck NZO transparent conductive film in this silicon substrate upper surface;
Step S4, on the described NZO transparent conductive film of previously preparation, evenly coating one deck colloidal sol rotates, and carries out anneal, to continue to form another layer of NZO transparent conductive film in the described NZO transparent conductive film upper surface of previously preparation;
Repeat step S4, wherein, the sodium/zine ion of the colloidal sol applied each time is than the sodium/zine ion ratio being all greater than previous primary coating colloidal sol.
2. the method for claim 1, is characterized in that, described stablizer is monoethanolamine solvent.
3. the method for claim 1, is characterized in that, described step S2 comprises:
Each described sample solution is carried out magnetic agitation 3h respectively under the constant temperature of 85 DEG C, to form colloidal sol corresponding to each described sample solution.
4. method as claimed in claim 3, is characterized in that, after forming colloidal sol corresponding to each described sample solution, also comprises and carries out still aging process to each described colloidal sol.
5. method as claimed in claim 4, it is characterized in that, the time of described still aging process is 48h.
6. the method for claim 1, is characterized in that, in described some sample solutions, sodium/zine ion ratio is respectively 1.5at%, 2.5at%, 4.0at%, 6.0at%, 8.0at%.
7. the method for claim 1, is characterized in that, step S3 specifically comprises:
The colloidal sol of the described sample solution of minimum sodium/zine ion ratio is evenly coated on the silicon substrate that rotating speed is 4000r/min and carries out rotation 30s, and 10min anneal under 350 DEG C of conditions is carried out to this colloidal sol.
8. the method for claim 1, is characterized in that, described two acetate hydrate zinc solutions, described ethylene glycol monomethyl ether solvent, described stablizer and described sodium hydrogen carbonate solution are analytical pure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510032546.XA CN104561941A (en) | 2015-01-22 | 2015-01-22 | Method for preparing NZO transparent conductive film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510032546.XA CN104561941A (en) | 2015-01-22 | 2015-01-22 | Method for preparing NZO transparent conductive film |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629284A (en) * | 2009-08-03 | 2010-01-20 | 北京航空航天大学 | Method for preparing aluminium-doped zinc oxide transparent conductive film by solvent thermal process |
| CN101994103A (en) * | 2009-08-17 | 2011-03-30 | 中国科学院理化技术研究所 | Preparation method of photoassisted sol-gel of yttrium doped zinc oxide transparent conductive film |
| CN102373425A (en) * | 2011-11-03 | 2012-03-14 | 浙江大学 | Method for preparing Na-doped p-type NnO film |
-
2015
- 2015-01-22 CN CN201510032546.XA patent/CN104561941A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629284A (en) * | 2009-08-03 | 2010-01-20 | 北京航空航天大学 | Method for preparing aluminium-doped zinc oxide transparent conductive film by solvent thermal process |
| CN101994103A (en) * | 2009-08-17 | 2011-03-30 | 中国科学院理化技术研究所 | Preparation method of photoassisted sol-gel of yttrium doped zinc oxide transparent conductive film |
| CN102373425A (en) * | 2011-11-03 | 2012-03-14 | 浙江大学 | Method for preparing Na-doped p-type NnO film |
Non-Patent Citations (5)
| Title |
|---|
| JIANUGO LÜ ET AL.: "Preparation and characterization of Na-doped ZnO thin films by sol-gel method", 《PHYSICA B》 * |
| SALIHA ILICAN: "Effect of Na doping on the microstructures and optical properties of ZnO nanorods", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| 周建等: "梯度掺杂AZO薄膜的制备及其性能表征", 《西南科技大学学报》 * |
| 李英伟: "掺钠对氧化锌薄膜p-型转变的研究", 《万方学位论文》 * |
| 谭伟石等: "《近代物理实验》", 30 September 2013 * |
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Application publication date: 20150429 |