EP2252728A2 - Elektrodepositionsverfahren zur herstellung von nanostrukturiertem zno - Google Patents
Elektrodepositionsverfahren zur herstellung von nanostrukturiertem znoInfo
- Publication number
- EP2252728A2 EP2252728A2 EP09711885A EP09711885A EP2252728A2 EP 2252728 A2 EP2252728 A2 EP 2252728A2 EP 09711885 A EP09711885 A EP 09711885A EP 09711885 A EP09711885 A EP 09711885A EP 2252728 A2 EP2252728 A2 EP 2252728A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- zno
- solution
- electrode
- electrode position
- nanostructured
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/08—Electroplating with moving electrolyte e.g. jet electroplating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
- C25D5/56—Electroplating of non-metallic surfaces of plastics
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
Definitions
- the invention relates to an electrode position method for producing nanostructured ZnO, in which in a standard three-electrode reactor, an aqueous solution of a Zn salt and a further component used and upon application of a potential and setting a deposition temperature of below 90 0 C on a in nanostructured ZnO substrate is deposited on the aqueous solution.
- Nanostructured ZnO material in the context of the invention is intended to mean ZnO in a morphology with dimensions in the nm range or less.
- the ZnO may be e.g. be formed in the form of nanorods, nanofilaments or thin layers. Due to its optoelectronic and environmentally friendly properties and its chemical stability, ZnO is promising materials for use in light emitting diodes and in highly structured solar cells.
- ZnO nanorods or nanofibers are produced by various methods.
- high deposition temperatures are typical. For instance, they are between 300 and 500 ° C. for the chemical vapor deposition (CVD) and metal organic chemical vapor deposition (MOCVD) processes, and between 400 and 500 ° C. for MOVPE (metal organic vapor phase epitaxy) processes. 600 to 900 0 C for the steam transport method and at about 900 0 C. for thermal vapor deposition.
- materials are deposited by means of electrodeposition methods and chemical bath deposition at moderate temperatures.
- the electrodeposition process is carried out at atmospheric pressure and is a low cost process which requires only simple equipment.
- the film thickness can be determined by means of the consumed charges during the deposition process.
- ZnO nanorods by means of electrodeposition methods are prepared from an aqueous solution, for example from a ZnCVKCl 2
- Electrolytic solution saturated with O 2 bubbles (described for example in 13th European Photovoltaic Solar Cell Energy Conference, 23-27 October 1995, Nice, France, pp 1750-1752 or in Appl. Phys. Lett., Vol. 77, No. 16, 16 October 2000, pp 2575-2577) or ZnO films of a ZnCl 2 / H 2 O 2 electrolyte solution as described, for example, in Journal of Electroanalytical Chemistry 517 (2001) 54-62.
- the nanostructured ZnO materials thus prepared do not have the properties such as high efficiency required for use in photovoltaics because photoluminescence spectra recorded for these materials show a very intense defect emission in the range of 450 to 900 nm as the main emission.
- IQE internal quantum efficiency
- the object is achieved by a method of the type mentioned above in that as a further constituent of the aqueous solution, a dopant for the nanostructured ZnO is used to improve the quality and the optical properties of the ZnO material.
- Zn (NO 3 ) 2 as Zn salt, in particular in a concentration of 1 to 20 mM.
- HNO 3 is used as a dopant, it is intended to prepare the aqueous solution of Zn (NO 3 ) 2 and HNO 3 in a molar ratio of about 100: 1, this solution having a pH of between 4.5 and 5.8 ,
- NH 4 NO 3 is used as a dopant, it is intended to prepare the aqueous solution of Zn (NO 3 ) 2 and NH 4 NO 3 in a molar ratio of from 1: 1 to 130: 1, this solution having a pH between 4.2 and 6.4 has.
- the method according to the invention has succeeded in producing ZnO nanorods with an average diameter of 100 to 280 nm by combining potentiostatic and galvanostatic processes manufacture.
- the ZnO nanorods show dominant band edge emission as desired and no additional annealing step, and have a high IQE, which is 23% and 28%, respectively, for the first ZnO nanorods deposited by the process.
- the measured high IQE showed deviations of 20 to 25%.
- IQE is one of the most important parameters for characterizing the quality of both light emitting and optoelectronic materials. It is defined as the ratio of the number of generated photons to the number of injected carriers. In general, the lower the defects in the material, the higher the IQE.
- a potential against the Pt reference electrode is set to a value between -1.2 V and -1.8 V, preferably between -1.3 V and -1.4 V.
- the deposition temperature between 60 0 C and 90 0 C is set and maintained over a period of a few minutes to 20 h.
- FTO SnO 2 : F
- ITO SnO 2 Mn
- Au Au
- Ag polymer with conductive coating or Si.
- Figure 1 Photoluminescence spectrum of ZnO nanorods prepared by electrodeposition from Zn (NOs) 2 ZH 2 O 2 , ZnCl or Zn (NO 3 ) 2 / NaOH electrolytes;
- FIG. 2 shows a scanning electron micrograph of ZnO nanorods produced by means of the method according to the invention with HNO 3 as dopant;
- FIG. 3 Photoluminescence spectrum of ZnO nanorods acc. Fig. 2; 4: further scanning electron micrograph of ZnO nanorods with altered morphology, produced by means of the method according to the invention with HNO 3 as dopant;
- FIG. 5 Photoluminescence spectrum of ZnO nanorods acc. Fig. 4;
- FIG. 6 Photoluminescence spectrum of ZnO nanorods of different diameters, produced by means of the method according to the invention with HNO 3 as doping agent.
- a glass substrate with a fluorine doped SnO 2 layer (so-called FTO glass), on which an undoped 30 nm thick ZnO layer is arranged, is used as the substrate.
- the substrate has a size of about 2.5 x 2 cm 2 and is first cleaned in an ultrasonic bath (acetone and ethanol) and then rinsing in distilled water.
- aqueous solution of 10 mM Zn (NO 3 ) 2 and HNO 3 with a pH of 4.5 is used in a mixing ratio of 100: 1 for the deposition.
- the solution is stirred.
- Typical deposition current densities in the process according to the invention are about 0.3 to 0.5 mA / cm 2 .
- the substrate was washed with the applied ZnO nanorods in distilled water.
- the morphology of the generated layers of ZnO rods was investigated by a scanning electron microscope (SEM).
- Photoluminescence measurements were carried out at an excitation wavelength of 325 nm (He-Cd laser).
- ZnO nanorods show the determined photoluminescence spectra of ZnO nanorods, for their preparation on an FTO glass substrate by means of electrode position method known from the prior art according to known electrolyte solutions (Zn (NOs) 2 ZH 2 O 2 , Zn (NO 3 ) 2 / NaOH, ZnCI) were used.
- Zn (NOs) 2 ZH 2 O 2 , Zn (NO 3 ) 2 / NaOH, ZnCI electrolyte solutions
- FIGS. 2 and 4 show images of the ZnO nanorods of different shapes produced by the method according to the invention with HNO 3 as a dopant.
- the different shapes are based on different potentials and molarities of the electrolyte solution.
- an IQE of about 28% was determined, for the 23% shown in FIG. 4.
- Fig. 6 shows the photoluminescence spectra at room temperature for ZnO nanorods with different diameters of about 100 nm to
- the different diameters were also realized by combining potentiostatic and galvanostatic techniques.
- the location of the intense maximum for band edge emission in the UV range and only a weak emission in the range of 450 nm to 700 nm, ie. the shape of the ZnO nanorods produced by the method according to the invention has no influence on their defect emission.
- the intensities of the photoluminescence spectra were indicated in the figures in arbitrary units.
- 10 mM Zn (NO 3 ) 2 and NH 4 NO 3 with a pH of 4.8 in a mixing ratio of 20: 1 are used as dopants and thus further constituents of the aqueous solution for the purpose of depositing nanostructured ZnO. All other details for carrying out the method according to the invention remain unchanged.
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Luminescent Compositions (AREA)
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102008010287A DE102008010287B3 (de) | 2008-02-21 | 2008-02-21 | Elektrodepositionsverfahren zur Herstellung von nanostrukturiertem ZnO |
DE200810029234 DE102008029234A1 (de) | 2008-06-19 | 2008-06-19 | Elektrodepositionsverfahren zur Herstellung von nanostrukturiertem ZnO |
PCT/DE2009/000254 WO2009103286A2 (de) | 2008-02-21 | 2009-02-20 | Elektrodepositionsverfahren zur herstellung von nanostrukturiertem zno |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2252728A2 true EP2252728A2 (de) | 2010-11-24 |
EP2252728B1 EP2252728B1 (de) | 2012-12-12 |
Family
ID=40941906
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP09711885A Not-in-force EP2252728B1 (de) | 2008-02-21 | 2009-02-20 | Elektrodepositionsverfahren zur herstellung von nanostrukturiertem zno |
Country Status (3)
Country | Link |
---|---|
US (1) | US20110048956A1 (de) |
EP (1) | EP2252728B1 (de) |
WO (1) | WO2009103286A2 (de) |
Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE202010018127U1 (de) | 2010-04-23 | 2014-04-04 | Helmholtz-Zentrum Berlin Für Materialien Und Energie Gmbh | Superstrat-Solarzelle mit Nanostrukturen |
DE102010017962A1 (de) | 2010-04-23 | 2011-10-27 | Helmholtz-Zentrum Berlin Für Materialien Und Energie Gmbh | Superstrat-Solarzelle mit Nanostrukturen |
JP2013525250A (ja) * | 2010-04-28 | 2013-06-20 | ビーエーエスエフ ソシエタス・ヨーロピア | 溶液中で亜鉛錯体を調製する方法 |
DE102010034904A1 (de) | 2010-08-18 | 2012-02-23 | Helmholtz-Zentrum Berlin Für Materialien Und Energie Gmbh | Zweiseitige Solarzelle |
DE102010034901B4 (de) | 2010-08-18 | 2016-06-02 | Helmholtz-Zentrum Berlin Für Materialien Und Energie Gmbh | Solarthermische Anordnung |
DE202010017656U1 (de) | 2010-08-18 | 2012-05-02 | Helmholtz-Zentrum Berlin Für Materialien Und Energie Gmbh | Zweiseitige Solarzelle |
CN102363893B (zh) * | 2011-11-02 | 2014-03-12 | 西南交通大学 | 一种同步合成两种ZnO纳米结构的方法 |
CN103194784B (zh) * | 2013-04-11 | 2016-03-02 | 江苏大学 | 一种以胶体为模板可控电沉积制备纳米ZnO薄膜的方法 |
DE102013113585A1 (de) | 2013-12-06 | 2015-06-11 | Helmholtz-Zentrum Berlin Für Materialien Und Energie Gmbh | Passivierungsschicht mit Punktkontakten für Dünnschichtsolarzellen |
DE102013113590A1 (de) * | 2013-12-06 | 2015-06-11 | Helmholtz-Zentrum Berlin Für Materialien Und Energie Gmbh | Verfahren zur Herstellung von Passivierungsschichten mit Punktkontakten für Dünnschichtsolarzellen |
WO2015081927A1 (de) | 2013-12-06 | 2015-06-11 | Helmholtz-Zentrum Für Materialien Und Energie Gmbh | Passivierungsschicht mit punktkontakten für dünnschichtsolarzellen und verfahren zu ihrer herstellung |
CN112903770B (zh) * | 2019-12-04 | 2022-05-17 | 中国石油化工股份有限公司 | 一种柔性硫化物产生菌菌量测定传感器及间接法测定污水中srb菌量的方法 |
CN114558592B (zh) * | 2022-03-09 | 2023-11-14 | 北方民族大学 | 一种ZnO/ZnS纳米棒核壳结构光催化剂及其制备方法 |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2732696B1 (fr) * | 1995-04-06 | 1997-06-20 | Centre Nat Rech Scient | Procede de preparation d'un film d'oxyde ou d'hydroxyde d'un element des colonnes ii ou iii de la classification, et les structures composites comprenant un tel film |
US5804466A (en) * | 1996-03-06 | 1998-09-08 | Canon Kabushiki Kaisha | Process for production of zinc oxide thin film, and process for production of semiconductor device substrate and process for production of photoelectric conversion device using the same film |
US6106689A (en) * | 1997-01-20 | 2000-08-22 | Canon Kabushiki Kaisha | Process for forming zinc oxide film and processes for producing semiconductor device substrate and photo-electricity generating device using the film |
JP3327811B2 (ja) * | 1997-05-13 | 2002-09-24 | キヤノン株式会社 | 酸化亜鉛薄膜の製造方法、それを用いた光起電力素子及び半導体素子基板の製造方法 |
US6160689A (en) | 1997-10-09 | 2000-12-12 | Jay Stolzenberg | Two wire solid state AC/DC circuit breaker |
US6576112B2 (en) * | 2000-09-19 | 2003-06-10 | Canon Kabushiki Kaisha | Method of forming zinc oxide film and process for producing photovoltaic device using it |
JP2002356400A (ja) * | 2001-03-22 | 2002-12-13 | Canon Inc | 酸化亜鉛の針状構造体の製造方法及びそれを用いた電池、光電変換装置 |
US20040016646A1 (en) * | 2002-07-29 | 2004-01-29 | Stucky Galen D. | Electrochemical synthesis of mesoporous metal/metal oxide flims using a low percentage surfactant solution by cooperative templating mechanism |
US20050189012A1 (en) * | 2002-10-30 | 2005-09-01 | Canon Kabushiki Kaisha | Zinc oxide film, photovoltaic device making use of the same, and zinc oxide film formation process |
JP2006324591A (ja) * | 2005-05-20 | 2006-11-30 | Nisshinbo Ind Inc | 電気二重層キャパシタ、その制御方法及びこれを用いた蓄電システム並びに二次電池 |
-
2009
- 2009-02-20 WO PCT/DE2009/000254 patent/WO2009103286A2/de active Application Filing
- 2009-02-20 US US12/918,747 patent/US20110048956A1/en not_active Abandoned
- 2009-02-20 EP EP09711885A patent/EP2252728B1/de not_active Not-in-force
Non-Patent Citations (1)
Title |
---|
See references of WO2009103286A2 * |
Also Published As
Publication number | Publication date |
---|---|
EP2252728B1 (de) | 2012-12-12 |
WO2009103286A2 (de) | 2009-08-27 |
US20110048956A1 (en) | 2011-03-03 |
WO2009103286A3 (de) | 2009-10-29 |
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