AT509400A1 - SOLUTIONS FOR THE MANUFACTURE OF HOMOGENOUS LARGE-SCALE PHOTOACTIVE LAYERS COMPRISING AN ELECTROACTIVE POLYMER AND SEMICONDUCTORING OPERATIONS AND THEIR APPLICATION IN PHOTOVOLTAICS AND OPTOELECTRONICS - Google Patents

Abstract

The invention is in the field of nanotechnology with a view to use in photovoltaics and optoelectronics. The process according to the invention makes it possible to produce semiconductor nanoparticles directly (in situ) in a wide variety of polymer matrices. The resulting nanocomposite layers can be used for the production of semiconductor devices, such as solar cells.

Description

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The invention is in the field of nanotechnology with a view to use in photovoltaics and optoelectronics. This method makes it possible to produce semiconductor nanoparticles directly (in situ) in a wide variety of polymer matrices. The resulting nanocomposite layers (mixture of inorganic nanostructures with a polymer) can be used for the production of semiconductor components such as solar cells (nanocomposite solar cells).

Nanocomposite solar cells are an alternative to inorganic solar cell technologies, as they can be produced more cost-effectively and energy-efficiently.1 The active layers of nanocomposite solar cells consist of inorganic nanostructures and electroactive polymers. As an inorganic nanoparticle component, materials such as CdSe, 2.3 CdTe4.5 CdS, 6 CIS, 7'8 CulnSe2.9'10 PbS, 11'12'13'14 PbSe, 15'16 HgTe, 17 Ti02.18, 1920,21 ZnO2223,24,2526 or (Zn, Mg) 027, but also modified fullerenes, for example PCBM, used.20'29'30'31,32'33'34,35'36 · 37 · 38 · 39 Als Polymer component can be used a variety of electroactive polymers.

Nanocomposite solar cells are built on two fundamental principles. On the one hand, a bilayer structure can be realized, wherein first a suitable electrode is coated with the inorganic semiconductor or the polymer component and only then the respective other component is applied. The disadvantage here is the small interface between the two components, at which the charge separation takes place. However, the subsequent transport of the charges to the respective electrodes is facilitated in this structure.

On the other hand, it is possible to use a bulk heterojunction structure, whereby the boundary layer between the two components is substantially increased compared to the bilayer structure, and a significantly larger number of free charge carriers can be generated. Due to the forming interpenetrating network of both components, however, the transport of the charge carriers to the electrodes is made more difficult. In general, however, solar cells with significantly higher efficiencies are obtained with this structure.

To realize a bulk heterojunction setup for nanocomposite solar cells, there are several methods. The process objective here is the production of thin layers of 100-500 nm, which consist of an interpenetriereriden network of two different classes of materials, namely inorganic semiconductors on the one hand, and polymers on the other hand.

On the one hand, a bulk heterojunction structure can be achieved by first having one of the two components (inorganic semiconductor component or polymer component) with a structure defined on one side Electrode is applied. For example, nanoparticles can be deposited as a porous layer as a first layer or nanostructures can be formed. 40, 41, 42 These structured layers are then filled with the respective other component and covered. This method is similar to the bilayer structure, but in this case a much larger interface between the two components is achieved.

Furthermore, it is possible to prepare nanostructures such as nanoparticles, nanorods, 43 nanodendrites, 44 special cases: modified fullerenes in a separate synthesis and then to mix them with an electroactive polymer in a suitable solvent. From the resulting solution, a layer is then applied to an electrode, forming a nanocomposite layer after evaporation of the solvent. The disadvantage here, however, that the inorganic nanostructures in the synthesis often long-chain stabilizers such as ligands or capper must be added to avoid agglomeration. However, these stabilizers prevent efficient charge separation at the interface between the inorganic semiconductor structure and the polymer component. By replacing the long-chain ligands with shorter-chain stabilizers prior to mixing with an electroactive polymer, this problem can at least be somewhat reduced.2,3

In part, this problem can be circumvented by synthesizing the nanoparticles directly in a polymer solution. However, the polymer does not stabilize the nanoparticles as effectively as long-chain ligands, which often leads to agglomeration of the nanoparticles. For example, lead sulfide nanoparticles have been synthesized in a polymer solution (MEH-PPV), which was subsequently applied to an electrode.11 45

In another method, inorganic nanostructures are produced directly in an electroactive polymer matrix (in situ). For this purpose, precursor compounds which by decomposition or reaction form nanostructures, such as nanoparticles, nanorods, nanodendrites, porous structures with holes in the nanometer range, hereinafter called nanostructure precursor compound, are dissolved together with an electroactive polymer in order to obtain a precursor solution. This solution is applied to a suitable electrode and the resulting nanostructure precursor compound / polymer layer is subsequently treated in such a way that nanostructures of the inorganic semiconductor component are formed directly in the polymer matrix.

This method has already been used for the direct production of oxidic46,47 and sulfidic48,48,50 nanostructures.

TiO 2 nanostructures were generated in an MDMO-PPV layer.51 Titanium isopropoxide was dissolved with MDMO-PPV in tetrahydrofuran, one layer was applied to one electrode, and then the TiO 2 precursor was converted into TiO 2 by hydrolysis. Furthermore, ZnO / MDMO-PPV nanocomposites were prepared by hydrolysis of diethylzinc.48,47

Binary sulfides, such as CdS, have been prepared by the reaction of Cd (N03) 2 with thioacetamide in a polyvinylpyrrolidone (PVP) matrix.52 However, this is a non-electroactive or conjugated polymer, which does not use such nanocomposite layers as active layers for solar cells can be.

An in situ method for the preparation of sulfidic semiconductors, e.g. CIS has been described.45 CIS nanoparticles were prepared in a PPV matrix from the metal salts, thioacetamide as the sulfur source, and a PPV precursor compound. In this case, however, a solvent mixture of polar solvents, such as pyridine, ethanol and water, must be used to prepare the precursor solution in order to be able to dissolve the respective metal salts and the sulfur source. This severely restricts the choice of useful electroactive polymers since they are typically soluble in apolar solvents. Furthermore, the application of homogeneous precursor layers to suitable electrodes due to the solvents used, e.g. high surface tension, and precursor compounds, for example, very different solubilities, extremely problematic.

These known methods show the following disadvantages: • very limited choice of solvents, since polar solvents, e.g. Water, are required for dissolving the metal salts and / or metal precursor compounds, • limited choice of electroactive polymers due to their low solubility in polar solvents, • limited choice of application methods of precursor solution on large-area substrates, as the high surface tension of aqueous or polar solvents Often, substrates are poorly wetted and homogeneous layer formation is therefore not possible. • Reaction by-products in the direct production of nanoparticles in the polymer matrix can only be insufficiently removed at temperatures at which electroactive polymers are typically stable. • Use of an additional chalcogenide squeeze.

The invention aims to remedy this situation.

The invention relates to a method for producing a coating solution comprising precursor compounds for metal chalcogenide nanostructures, which is characterized in that compounds in one or more organic solvents are dissolved as precursor compounds for the metal chalcogenide nanostructures and can be converted by energy input into metal chalcogenide nanostructures.

Further advantageous embodiments of the method according to the invention are disclosed in claims 2 to 8.

The invention further relates to the production of nanocomposite layers using the coating solutions prepared according to the invention in conjunction with at least one electroactive polymer with energy input.

This manufacturing method according to the invention is disclosed in claims 9 to 19.

The invention also relates to the use of these nanocomposite layers for producing components or components, such as solar cells, sensors or detectors, electrical or optical components comprising UV, IR and microwave regions, switches, displays or radiation-emitting components, such as lasers or light-emitting components Diodes (LEDs).

The technical problem that can be solved with this invention relates to the production methods for bulk heterojunction solar cells. The known preparation of the precursor solution for this method is difficult, since typically the precursor compounds for the semiconductor manoparticles in polar, and the electroactive polymers are better soluble in apolar solvents.

The central point of the invention presented here is that the possibility is created of preparing precursor solutions of nanostructure precursor compounds and electroactive polymers which are more soluble in apolar solvents. This is made possible by the fact that the necessary metal compounds for the formation of nanoparticles are chemically modified so that they can be solved as nanostructure precursor compound in many common organic solvents.

Furthermore, the nanostructure precursor compounds convert at low temperatures, i. below 400 eC, preferably below 200 ° C, or low energy input into the Halbleitemanostrukturen within the polymer matrix to, and thus a thermal degradation of the electroactive polymer is prevented. ·· * »t * 5 * ·»

Due to the good solubility of the nanostructure precursor compounds in a wide variety of solvents, the use of many electroactive organic compounds which are soluble in these solvents is possible as a second component for the preparation of nanocomposite layers.

The use of these particular nanostructure precursor compounds (for example: metal thiocarbamates, metal dithiocarbamates, metal thiocarboxylates, metal dithiocarboxylates, metal xanthates, metal trithiocarbonates, metal thiolates, metal thiocyanates and / or metal isothiocyanates) also allows the preparation of a solution with these compounds and the electroactive polymer in a wide concentration range.

In the case of the production of metal chalcogenide nanostructures, no external chalcogenide source for preparing the metal chalcogenide nanostructures of the solution must also be added since the chalcogenide source is already present in the precursor compound. As an external source of chalcogenide, compounds are understood which additionally provide elements of the 6th main group when the energy is introduced or when the metal chalcogenide nanostructures are formed.

Another advantage is that the chalcogenide source in the precursor compound is already in close proximity to the metals, facilitating the reaction to form the semiconductor structure. This method also makes it possible to produce very pure semiconductor nanostructures.

By chemical modification of the nanostructure precursor compounds their solubility can be greatly influenced, whereby the production of precursor solutions in a variety of solvents and solvent mixtures is made possible. Specifically, typical solvents for electroactive polymers (organic solvents such as: chloroform, toluene, chlorobenzene, tetrahydrofuran, xylene) can be used. Consequently, many common electroactive polymers can be used to make nanocomposite layers and nanocomposite solar cells. Furthermore, the properties of the precursor solution (viscosity, boiling point, surface tension, etc.) can be varied over a wide range by selecting the solvent or solvent mixture and suitable nanostructure precursor compounds, thus widening the selection of application methods of the precursor solution, especially for large-area substrates.

A big advantage compared to other methods is that a large amount of metal compounds (metafl-sulfur precursors) can be dissolved together with an electroactive polymer. It can be achieved solutions with high metal content but also with high polymer content. 6 • · · · · · · · · · · «· · · · · · · · · · · · · · · · · · · * • Φ ·

Thus, the viscosity of the solution can be adjusted well, which in turn widens the spectrum of different application methods or coating methods. By changing the viscosity of the solution, the layer thickness of the applied layer can also be adjusted.

Due to the excellent solubility of the components in organic solvents is a very good processability and a homogeneous distribution of the components in the precursor solution, and subsequently after the layer application in the layer, given.

By choosing the solvent, both rough and smooth layers can be achieved. The use of very low boiling volatile solvents promotes the formation of rough layers, while the use of less volatile, higher boiling solvents enables the production of very smooth layers.

The resulting nanocomposite layers are characterized by a high purity, since the resulting reaction by-products are volatile and thus can be removed from the nanocomposite layer even at very low temperatures.

It is not obvious to the invention that all necessary nanostructure precursor compounds can be modified to such an extent that they are soluble in organic solvents in which organic electroactive compounds can also be dissolved. Furthermore, it is not obvious that with solutions containing a high proportion of these nanostructure precursor compounds and an electroactive polymer, homogeneous large-area layers can be applied to suitable substrates and these can be converted by controlled energy input to nanocomposite layers. In addition, it is not obvious that nanoparticles in the size range between 3 and 30 nm form, which form differently pronounced interpenetrating networks depending on the concentration ratio of the nanostructure precursor compounds to the electroactive polymer.

The main advantages of the described method are listed in the following list: • simple chemical modification of the nanostructure precursor compounds and associated solubility of the nanostructure precursor compounds in organic solvents, in which organic electroactive compounds can be solved • wide range of organic solvents, in which electroactive polymers are soluble, for the preparation of the precursor solution. *** · * Φ Φ · · · · · · Φ · 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7. * • * * * * * ft *·· ··· ···· Boiling point, viscosity, surface tension, etc.) can be varied within a wide range. • Wide range of application methods of precursor solution to large area substrates. • Reaction byproducts of direct preparation of nanoparticles in the polymer matrix can be well removed at temperatures where electroactive polymers are typically stable become.

The following examples give an overview of possible areas in which this invention can be realized.

Solutions were prepared with a wide variety of combinations of nanostructure precursor compounds for the preparation of the semiconductor structures and electroactive polymers in numerous solvents or solvent mixtures with different concentration ratios.

Furthermore, nanocomposite layers containing different electroactive polymers (for example: MEH-PPV, MDMO-PPV, F8T2, P3HT) and inorganic semiconductors (for example: copper indium disulfide (CIS), zinc sulfide-copper indium disulfide (ZnS-CIS), copper zinc tin sulfide (CZTS )) produced. The energy input for converting the precursor layers into the nanocomposite layers was carried out thermally (heating plate or IR radiation) or else by radiation (electron beam). The characterization of these layers showed that nanoparticles in the size range between 3 and 30 nm are formed, which, depending on the concentration of the nanostructure precursor compounds, form differently pronounced interpenetrating networks. Solar cells with these nanocomposite layers as active layers achieved efficiencies above 1.7%. Measurements of the spectral sensitivity of these solar cells showed that the semiconductor structures contribute significantly to the generation of charge carriers in the active layer.

Examples:

Example 1: Synthesis of Cu, In and Zn xanthates

The synthesis of the different Cu, In and Zn xanthates is shown in Figure 1. In the first step, the desired alcohol is reacted with carbon disulfide in the presence of a base (e.g., potassium hydroxide or potassium ferf-butoxide) to give the corresponding potassium xanthate53. In the second step, the corresponding potassium xanthate is then reacted with a source of Cu, In, or Zn54.

Mn + salt + η Κ S ^ S 2. Ο. 1 t + Μ Κ salt + Μ

koh + cs2 + r-oh

Figure 1: Schematic diagram of the synthesis of Cu, In, and Zn xanthates

Figure 2 summarizes examples of synthesized Cu, Zn and Zn xanthates wherein the substituents R, R2 and R3 represent alkyl groups in substituted, unsubstituted, branched and straight chain form and are abbreviated, for example, as follows: Et = -ethyl, amyl = -amyl, Dec = -decyl, HepB = -2,4-dimethyl-3-pentyi, Hex = -3,3-dimethyl-2-butyl, Hep = -2,2-dimethyl-3-pentyl, HepC = 4,4-dimethyl-pentyl, OHep = -1-tert-butoxy-2-propyl, PhEt = -1-phenyl-1-propyl.

✓X'X

Hep HepC OHep PhEt

Figure 2: Examples of synthesized Cu, In, and Zn xanthates

Figure 3 gives examples of synthesized Cu, In and Zn xanthates that are not yet known in the literature. Depending on the metal used and the R radical chosen, the solubility of the resulting xanthate is very different. In (III) - and Zn (II) xanthates generally have a very good solubility in contrast to Cu (l) xanthates, since they can due to the higher metal valencies more xanthate groups, which cause a better solubility carry. 9 ·· 4 ··· • 4 • * 4 • I · # «4 4 4 t · ·· 4 ·

yV HepB

HepC OHep PhEt Figure 3 shows synthesized and unknown in the literature Cu, In and Zn xanthates, where R, R3 and R2 and HepB, Hex, Hep, HepC, OHep and PhEt have the definition and nomenclature listed in Figure 2 , R =

Example 2 Synthesis of Cu and In Dithiocarbamates

The synthesis of in, and Cu dithiocarbamates is similar to the xanthat synthesis and is briefly described below. In the first step, the desired amine and carbon disulfide are reacted in the presence of a base (e.g., sodium hydroxide) to give the corresponding sodium dithiocarbamate 55,56. Thereafter, the sodium dithiocarbamate is reacted with a Cu or In source to obtain the corresponding In, and Cu dithiocarbamate.

Figure 4 shows an example of a synthesized Cu and In dithiocarbamate, namely copper 2-hexyldithiocarbamate and indium-2-hexyldithiocarbamate.

10 «· ·» • · ♦ · • · ♦ · • ♦ · · · * Μ ··· ·

Example 3: Synthesis of Sn xanthates

In the synthesis of Sn xanthates, the choice of solvent determines the major product obtained. For example, when tin tetrachloride is reacted with potassium xanthate in benzene, SnExa4 is obtained. However, using methanol or ethanol, Sn2S2Exa4, a Sn-xanthate bridged by 2 sulfur, is the major product.

Figure 4 gives examples of synthesized Sn xanthates.

SnExa4 Sn2S2Exa4 Sn2S2Hex4

Figure 4 shows the synthesized Sn xanthates, namely SnExa4 = tin ethylxanthate, Sn2S2Exa4 = tin diethylxanthate and Sn2S2Hex4 = tin thio-dihexylxanthate.

EXAMPLE 4 Production of Copper Indium Disulfide / Polymer Nanocomposite Layers by Different Application Methods For the precursor solution for producing the nanocomposite layer, the respective Cu (I) xanthate and In (III) xanthate were mixed in the desired Cu / In ratio in a solvent or Solvent mixture dissolved. The clear precursor solution was then applied to a glass iTO substrate by a suitable deposition method. In order to obtain the copper indium disulfide / polymer nanocomposite layer (CIS / polymer nanocomposite layer), the substrate with the previously applied precursor layer was annealed for 15 minutes at 200 ° C at a heating rate of 21 ° C / min. Accordingly, the preparation of the CIS nanoparticles from the Cu and In xanthates occurs within the matrix of the conjugated polymer in situ during this heating step.

Figure 5 shows a diffractogram of a CIS / poly (2- (2-ethylhexy! Oxy) -5-methoxy-p-phenylenevinylene nanocomposite layer (CIS / MEH-PPV nanocomposite layer) in which the solution was applied by spraying are shown in Table 1. The three broad reflections at 28.1 ° (112), 46.5 ° (204/220) and 54.9 ° (312) are characteristic of copper indium disulfide in the chalcopyrite structure 3 nm, calculated according to the Scherrer equation with the two most intense reflections 11 11 φ φ φ φφ φ φφ ··· φ ♦ • · I · · · · · · «φ φ φ ·· φ φ φ φ 4 · · *** "· 4 Φ * ΦΦ · · Φ *

Figure 5: X-ray diffraction pattern of a CIS / MEH-PPV nanocomposite layer

Similarly, a CIS / poly-co- (dioctylfluorenyl-dithiophenyl) nanocomposite layer (CIS / F8T2 nanocomposite layer) was also prepared by spin-coating the precursor solution. Detailed production parameters are again given in Table 1. Figure 6 shows a TEM (Transmission Electron Image) image of this photoactive nanocomposite layer. The nartoparticles (dark areas) are embedded in the polymer matrix and have an approximate size of 5 nm.

Furthermore, the photoactive nanocomposite layer can also be applied to a glass ITO substrate by doctoring. In this connection, reference is made to Example 9 in which solar cells were produced by this application method.

Table 1: Detailed production parameters for the preparation of ClS / polymer nanocomposite layers..... · · · · · · · * * * * · · · · 12 · · · · · · »

Example 1 2 Polymer MEH-PPV F8T2 Cu-Xanthat Cu-Amyl Cu-Hex In-Xanthat In-Eta Ιη-Ηβχ ^ Cu / In Ratio 1 / 1.7 1 / 1.7 CIS / Polymer Ratio 3/1 4/1 Solvent CHCla / Pyridines (1 / 0.25) CHCI3 Method of application Spray Spin coats

The abbreviations used in Table 1 have the following meaning: MEH-PPV = Pdy (2- (2-ethylhexyloxy) -5-methoxy-p-phenylenevinylene), F8T2 = poly-co- (dioctylfluorenyl-dithiophenyl), Cu-amyl = Kupferamylxanthat , Cu-Hex = copper-3,3-dimethyl-2-butylxanthate, In-Et3 = indium ethylxanthate, In-Hex3 = indium-3,3-dimethyl-2-butylxanthate, CHCl3 = chloroform.

Example 5: Preparation of CIS / Polymer Nanocomposite Layers by Different Conversion Methods

One way to form the CIS / polymer nanocomposite layer is to heat the precursor layer in a tube furnace. As an example of this, the CIS / F8T2 nanocomposite layer cited under Example 4 can be used. In this case, the precursor layer was annealed for 15 minutes at 200 ° C at a heating rate of 21 ° C / min in a tube furnace.

In addition, the conversion of precursor to CIS can also be effected by high-energy radiation, such as an electron beam. In Figure 7 and Figure 8, the diffraction patterns and associated radial intensity profiles of a CIS / poly [2-methoxy-5- {3,7-dimethyloctyloxy)] p-phenylene vinylene nanocomposite layer (CIS / MDMO-PPV nanocomposite layer ) after different exposure of the electron beam to the precursor layer.

The electron beam of a transmission electron microscope (TEM) usually has an energy of 100-300 keV. In particular, this can lead to polymer damage to the sample due to the energy input. In the course of these experiments it was investigated whether the transformation of the xanthates is also possible by the energy of the electron beam. 13 00 0000 0 0 · 0 0 0 ·· ·· ·· · • 0 0 0 0 ·· # · ♦ · · t · f 0 0 0 · 0 0 *

A B

Figure 7: TEM diffraction patterns after irradiation for Os (A) and 800s (B)

A B Figure 8: Radial intensity profiles (A) of the diffraction images shown in Figure 7 and enlarged image (B).

For this purpose, a film was prepared by spin-coating on a NaCl monocrystal, dissolved in aqua dest and measured as a TEM sample. A sample site was illuminated with the electron beam and observed in the diffraction mode.

Figure 7 shows the diffraction patterns at the beginning of the experiment and after an exposure time of 800s. The formation of individual rings is clearly recognizable. Figure 8 shows the radial intensity gains of the diffraction patterns. The formation of CIS can be observed and demonstrated by the two resulting peaks characteristic for CIS. »· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

Figure 9: TEM image of the nanoparticles in the layer after irradiation of the sample (A), optical image of the irradiated sample site (B) •······· 9 99 9

After the experiment, as shown in Figure 9, the formed CIS nanoparticles could also be imaged by TEM without further alteration of the sample. The particle size is in the range of 2-3 nm. In the optical microscope, the irradiated area was recognizable due to the color change of the film.

Example 6: Preparation of a copper zinc tin sulfide / MDMO-PPV nanocomposite layer

To obtain the copper zinc tin sulfide / MDMO-PPV nanocomposite layer (CZTS / MDMO-PPV nanocomposite layer), a NaCl single crystal! coated with the precursor solution and then annealed for 15 minutes at 200 ° C at a heating rate of 21 ° C / min (more precise Hersteliungsparameter are listed in Table 2.

Table 2: Manufacturing parameters of the CZTS / MDMO-PPV nanocomposite layer

Polymer MDMO-PPV Cu-Xanthat Cu-Hex Zn-Xanthat Zn-Hex Sn-Xanthat Sn2S2Hex2 Cu / Zn / Sn Ratio 2/1/1 CZTS / Polymer Ratio 4/1 Solvent CHCl3 Application Method Spin coats

Figure 10 shows a TEM image and a diffraction pattern of this CZTS / MDMO-PPV nanocomposite layer. The radial intensity profile calculated from this corresponds to that of 15 × fl • • · · fl • • • # # # # # # # # # #.

Kupferzinkzinnsulfid. Accordingly, the preparation of the CZTS nanoparticles from the Cu, Zn and Sn xanthates occurs within the matrix of the conjugated polymer in situ during this heating step. r) SlilBI eiii '; Uj ^ r ,: τ! 0 ·! !?! *! ί · !! ί "1 ϊ ·! ι '\ ^ · ίί! μΜ u. 1 μιτι 5 1 / i ü \ I_5

Figure 10: TEM image of the CZTS / MDMO-PPV nanocomposite layer (a), the marked area was used for the electron diffraction, diffraction pattern of the selected sample location (b), radial intensity profile created from the diffraction image (c)

Example 7: Preparation of a CIS / MDMO-PPV nanocomposite solar cell: For the precursor solution for the preparation of the nanocomposite layer, Cu (I) heptylxanthate and In (111) -hexy-xanthat were in a molar ratio of 1 / 1.7 in chloroform solved. The resulting solution was then added to MDMO-PPV. When the Cu and In xanthates are completely converted to copper indium disulfide, the ratio CIS / MDMO-PPV corresponds to 4.5 / 1 in the photoactive nanocomposite layer. The clear precursor solution was then applied to a suitable substrate. In order to obtain the CIS / MEH-PPV nanocomposite layer, the substrates were annealed with the previously applied precursor layer for 15 minutes at 200 ° C. As a last step, calcium / aluminum was then vapor-deposited as a cathode material onto the photoactive nanocomposite layer.

The basic structure of a solar cell is shown in Figure 11. On a glass substrate (1) is a transparent indium tin oxide (ITO) electrode (2), which serves as an anode. The photoactive nanocomposite layer (3) is then produced on this structure and then the cathode (4) is applied. In order to obtain a closed circuit, the contacting takes place via anode and cathode. 16 "• • • ftftftftft! ·············································

Figure 11: Basic structure of a CIS / polymer hybrid solar cell; (1) glass substrate, (2) indium tin oxide (ITO) electrode, (3) photoactive nanocomposite layer, (4) cathode

A representative current / voltage characteristic is shown in Figure 12. The open cell voltage (V0c) is 510 mV and the short-circuit current (lsc) is 5.79 mA / cm2. The fill factor (FF) of 44.6% results in a calculated efficiency (η) of 1.0%.

Voltage [V] Figure 12: Current / Voltage characteristic of a CIS / MDMO PPV solar cell

Example 8: Preparation of CIS / polymer solar cells with different photoactive polymers

Simultaneously with the production of the CIS / MDMO-PPV solar cell described above, further nanocomposite solar cells were produced with other conjugated polymers.

Table 3 gives an overview of possible combinations and the results obtained therewith. 17

Table 3: Tested photoactive polymers for the preparation of CIS / polymer solar cells

Example 1 2 3 4 5 6 Polymer PF-Gly F8BT F8T2 P3EBT P3HT MEH-PPV Cu-Xanthat Cu-Amyl Cu-Amyl Cu-Amyl Cu-Amyl Cu-Amyl Cu-Amyl In-Xanthat In-Et3 In-EU In Et3 In-Et3 In-Et3 In-Et3 Cu / In ratio 1 / 1.7 1 / 1.7 1 / 1.7 1 / 1.7 1 / 1.7 1 / 1.7 CIS / polymer ratio 3/1 3/1 3/1 2/1 2/1 4/1 VocM 0,202 0,520 0,377 0,533 0,221 0,65 Isc [mA / cm *] 2,41 0,72 0,84 0,52 0,08 1 , 66 FF [%] 29.0 26.9 28.1 28.0 24.7 33.5 Π [%] 0.14 0.10 0.09 0.08 0.005 0.35 PF-Gly: poly ( 9,9-di {2- [2- (2-methoxyethoxy) ethoxy] ethyl} fluorenyl-2,7-diyl) F8BT: poly [(9,9-di-n-octylfluorenyl-2,7-diyl ) -a / f- (benzo [2,1,3-thiadiazole-4,8-diyl)] P3EBT: poly [3- (ethyl-4-butanoate) thiophene-2,5-diyl] P3HT: poly (3-hexylthiophene -2,5-diyl)

Example 9: Preparation of Zinc Sulfide CIS / Polymer Solar Lines

Furthermore, it is also possible by adding Zn-xanthate to form zinc sulfide-CIS mixed phases (ZnS-CIS mixed phases). The influence of such mixed phases on the properties of a ZnS-CIS / F8T2 solar cell is shown in Table 4. Up to a Cu / Zn ratio of 1 / 0.1 there is a significant improvement of the short-circuit current and the fill factor and thus an increase in the efficiency up to 0.59%.

Table 4: ZnS-CIS / F8T2 solar cells with different proportions of ZnS

Example 1 2 3 4 5 6 7 Cu-Xanthat Cu-Hex Cu-Hex Cu-Hex Cu-Hex Cu-Hex Cu-Hex Cu-Hex In-Xanthat In-Hex3 In-Hex3 In-Hex3 In-Hex3 In-Hexs In-Hex3 In-Hex3 Zn-Xanthat Zn-Hex2 Zn-Hex2 Zn-Hex2 Zn-Hex2 Zn-Hex2 Zn-Hex Zn-Hex2 Cu / In Ratio 1 / 1.7 1 / 1.7 1 / 1.7 1 / 1.7 1 / 1.7 1 / 1.7 1 / 1.7 Cu / Zn ratio 1/0 1 / 0.05 1 / 0.1 1 / 0.15 1 / 0.4 1 / 1 1 / 1.5 Voc [V] 0.42 0.4 0.45 0.35 0.36 0.47 0.51 Isc [mA / cm 2] 2.75 3.39 3.74 3.22 3 , 36 1,57 0,76 * ° * · · · · · · · »M« * »·» * * · · · · · «*» · ♦ # «ι · ♦ · FF [%] 33,7 35 , 0 35.1 32.15 27.4 28.0 25.6 n [% I 0.39 0.47 0.59 0.36 0.32 0.20 0.10

Example 10: Preparation of CIS / polymer solar cells with different solvents

Due to the excellent solubility of the described Cu and In precursor, a number of different organic solvents in a mixture or pure can be used for the preparation of the precursor solution. As a result, the morphology of the resulting CIS / polymer nanocomposite layer can be selectively altered and the efficiency of the solar cells greatly influenced.

Table 5 and Table 6 give an exemplary overview of possible solvents and solvent combinations for making a CIS / F8T2 solar cell and a CIS / MEH-PPV solar cell.

Table 5: Influence of different solvents and solvent combinations on the parameters of CIS / F8T2 solar cells

Example 1 2 3 4 5 solvent CHCl 3 THF chlorobenzene dichlorobenzene CHCl 3 / THN 0.9 / 0.1 Cu-xanthate Cu-hex Cu-Hep Cu-Hep Cu-Hep Cu-Hep In-Xanthate In-Hex 3 In-Hep 3 In Hep3 In-Hep3 In-Hep3 Cu / In Ratio 1 / 1.7 1 / 1.7 1 / 1.7 1 / 1.7 1 / 1.7 ClS / Polymer Ratio 4/1 4/1 4 / 1 4/1 4/1 VOC [V] 0,57 0,33 0,47 0,29 0,33 ISC [mA / cm2] 3.71 1,09 4,28 2,98 0,60 FF [%] 31 , 2.29.8 21.7 38.8 29.8 n [%] 0.66 0.11 0.44 0.34 0.11 THF: tetrahydrofuran THN: tetrahydronaphthalene t9 ::

Table 6: Influence of different solvents on the parameters of CIS / MEH-PPV solar cells

Example 1 2 CHCI3 solvent toluene Cu-xanthate Cu-Hep Cu-Hep In-Xanthate In-Hep3 In-Hepa Cu / in ratio 1 / 1.7 1 / 1.7 CIS / polymer ratio 4.5 / 1 5 / 1 Voc [V] 0.53 0.33 Uc [mA / cm ^] 2.89 1.06 FF [%] 32.7 27.1 rj [%] 0.50 0.16

Figure 13 shows the Incident-Photon-to-Electron Conversion Efficiency spectrum (IPCE spectrum), where the photocurrent is measured spectrally, and the absorption spectrum of the CIS / MEH-PPV solar cell from Table 6 / Example 1. The increase in absorption in the 850nm to 600nm range is mainly due to the CIS nanoparticles. From about 600 nm MEH-PPV begins to absorb, which is reflected in a pronounced increase in absorption. From the comparison of the IPCE spectrum and the absorption spectrum, it can be seen that the inorganic nanoparticles clearly contribute to the generation of electricity. Even outside the absorption range of the polymer {> 600 nm) there is a considerable increase in the IPCE curve starting with the absorption beginning of the nanoparticles at about 850 nm.

Figure 13: IPCE and absorption spectrum of a CIS / MEH PPV solar cell 20 • · • ·

Example 11: Preparation of CIS / polymer solar cells with different Cu / In ratios

By varying the ratio of Cu-xanthate to In-xanthate, the properties of the forming CIS nanoparticles and the resulting nanocomposite layer can be influenced.

Table 7 gives an overview of the influence of the Cu / In ratio on the parameters of CIS / F8T2 solar cells.

Table 7: Influence of the Cu / In ratio on the parameters of C IS / F8T2 solar cells

Example 1 2 3 4 5 Solvents CHCl3 CHCl3 CHCl3 CHCl3 chci3 Cu-Xanthat Cu-Hex Cu-Hex Cu-Hex Cu-Hex Cu-Hex In-Xanthate In-Hex3 In-Hex3 In-Hex3 In-Hex3 In-Hex3 Cu / In ratio 1 / 1.9 1 / 1.7 1 / 1.6 1 / 1.5 1 / 1.3 ClS / polymer ratio 4/1 4/1 4/1 4/1 4/1 VocM 0 , 3 0.55 0.31 0.45 0.02 Isc EmA / cm *] 3.69 3.65 2.37 2.90 1.00 FF [%] 29.3 30.1 26.6 27, 6 35.0%] 0.38 0.66 0.26 0.57 0.01

Example 12: Preparation of CIS / polymer solar cells by means of doctoring

Another advantage in the use of a wide variety of solvents is that properties such as viscosity, boiling point, solubility of the precursor, etc., can be precisely adjusted and thus a wide range of application methods for the precursor layer is available. In contrast to spincoating, which is limited to quite small substrates, even large-area substrates can be uniformly coated with the precursor solution during doctor blading.

Table 8 gives the average efficiencies of CIS / polymer solar cells along a substrate measuring 7cm x 4cm, as shown schematically in Figure 14. * 1 • · · * «• #» φ # · • φ · * · φφφ φ • · · · • φφ ·

ε ο S 4 - * 4 cm 1: glass substrate 2: indium tin oxide layer 3: photoactive nanocomposite layer 4: cathode

Figure 14: Distribution of CIS / polymer solar cells along a substrate, where the precursor solution was applied by doctoring

Table 8: Average efficiencies of CIS / polymer solar cells where the precursor layer was applied by doctoring

Example 1 2 Polymer F8T2 MDMO-PPV Solvent CHCl 3 Chlorobenzene Cu-Xanthate Cu-Hex Cu-Hep In-Xanthate In-Hex 3 In-Hep 3 Cu / In Ratio 1 / 1.7 1 / 1.7 CIS / Polymer Ratio 4 / 1 4.5 / 1 VocM 0.54 0.60 Isc [mA / cm *] 2.89 6.89 FF [%] 25.7 41.3 Π [%] 0.41 1.31

Example 13 Preparation of CIS / Polymer Solar Cells with Dithiocarbamates as Cu and In Precursor

In addition to xanthates, dithiocarbamates can also be used to prepare CIS / polymer solar cells. Figure 15 shows the characteristics of a CIS / MEH PPV solar cell based on Cu and ln dithiocarbamates. In the precursor solution, the Cu / In ratio was adjusted to 1/1/7 and the CIS / polymer ratio was set to 1/3 and used as the solvent chloroform. 22 * «· * · • ·

Figure 15; Current-voltage characteristic of a CIS / MEH PPV solar cell based on Cu and in-dithiocarbamates

2-theta scale

Figure 16: XRD of a CIS layer made of Cu and in-dithiocarbamates XRD diffractogram

Figure 16 shows an X-ray diffractogram of a CIS layer prepared from Cu and in-dithiocarbamates. In addition to stoichiometric CIS, an indium-rich phase is also formed. The 3 most intense peaks at 28 °, 46 ° and 55 ° 2Θ agree with the most intense peaks of stoichiometric CIS (PDF 01-075-0106). The weaker peaks at 32 °, 44 °, 58 °, 68 "and 75 ° 2Θ are also from stoichiometric CIS. The peaks at 23 °, 33 °, 41 °, 48 ", 60 ° and 80β 2Θ most likely originate from indium-rich copper indium sulfide InisjCuo.geCui.ge ^ (PDF 01-081-0785). The peaks at 28 °, 44 °, 68 °, 71 °, 77 ° 2 ° can originate from both materials.

On the basis of the synthesized routes and the analysis data prepared in this context, it can be shown that very efficient nanocomposite structures, which are powerful components for the field of photovoltaics and optoelectronics, can be provided in a procedurally uncomplicated solution. «« ··· «« «···« • ·} 4 ·· ψ · · ο «· · · · · ·························································

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Claims (20)

1. A process for the preparation of a coating solution comprising precursor compounds for metal chalcogenide nanostructures, characterized in that are dissolved as precursor compounds for the metal chalcogenide nanostructures compounds in one or more organic solvents and walls by energy input in metal chalcogenide nanostructures , 2. A method for producing a coating solution comprising precursor compounds for metal chalcogenide nanostructures, characterized in that as precursor compounds for the metal chalcogenide nanostructures compounds in one or more organic solvents, preferably in the presence of a photoactive polymer, are dissolved and by energy input in metal chalcogenide nanostructures let convert. 3. A process for the preparation of a coating solution comprising precursor compounds for metal chalcogenide nanostructures, characterized in that as precursor compounds for the metal chalcogenide nanostructures compounds in one or more organic solvents, preferably in the presence of a photoactive polymer, and dissolved by energy input without additional chalcogenide in To convert metal chalcogenide nanostructures. 4. A process for preparing a coating solution comprising precursor compounds for metal chalcogenide nanostructures, characterized in that two or more precursor compounds for the metal chalcogenide nanostructures in one or more organic solvents, preferably in the presence of a photoactive polymer, are dissolved and by energy input depending on the used Convert the amount into different metal chalcogenide nanostructures or metal chalcogenide nanostructures with different stoichiometry. 5. A process for the preparation of a coating solution comprising precursor compounds for metal chalcogenide nanostructures, characterized in that two or more precursor compounds for the metal chalcogenide nanostructures are dissolved in one or more organic solvents, preferably in the presence of a photoactive polymer, and transformed into ternary energy by convert quaternary and / or higher metal chalcogenide nanostructures. I · t ································································································································································································· 6. A process for producing a coating solution comprising precursor compounds for metal chalcogenide nanostructures, characterized in that as precursor compounds for the metal chalcogenide nanostructures compounds selected from the group of thiocarbamates, dithiocarbamates, thiocarboxylates, dithiocarboxylates, xanthates, trithiocarbonates, thiolates, thiocyanates and / or isothiocyanates be synthesized and dissolved in one or more organic solvents, preferably in the presence of a photoactive polymer, and can be converted by energy input into metal chalcogenide nanostructures. 7. A process for producing a coating solution comprising precursor compounds for metal chalcogenide nanostructures, characterized in that two or more precursor compounds for the metal chalcogenide nanostructures compounds selected from the group of thiocarbamates, dithiocarbamates, thiocarboxylates, dithiocarboxylates, xanthates, trithiocarbonates, thiolates, thiocyanates and / or isothiocyanates are synthesized and dissolved in one or more organic solvents, preferably in the presence of a photoactive polymer, and can be converted by energy input into ternary, quaternary and / or higher metal chalcogenide nanostructures. 8. A process for the preparation of a coating solution according to one or more of claims 1 to 7, wherein it is prepared without additional chalcogenide. 9. Production of nanocomposite layers from layers applied from solutions according to one or more of claims 1 to 7 and at least one electroactive polymer by energy input. 10. Production of nanocomposite layers from layers applied from solutions according to one or more of claims 1 to 7 and an electroactive polymer, wherein the nanostructures are produced directly in the applied layer, consisting of nanostructure precursor compounds and electroactive polymer, by energy input. 11. Preparation of nanocomposite layers by thermal treatment of layers applied from solutions according to one or more of claims 1 to 7 and an electroactive polymer. 12. Preparation of nanocomposite layers by thermal treatment of layers applied from solutions according to one or more of claims 1 to 7 and an electroactive polymer, the nanostructures being applied directly in the applied v > • ······················································································································································································································································· Polymer, to be produced. 13. Preparation of nanocomposite layers according to one or more of claims 9 and 12, wherein the layers applied from solutions according to one or more of claims 1 to 7 and an electroactive polymer with radiation, in particular high-energy radiation, such as electron beam, X-radiation or microweElenstrahlung is treated , 14. Preparation of nanocomposite layers by thermal treatment of layers applied from solutions according to one or more of claims 1 to 7 and an electroactive polymer, wherein the temperature in the layer does not exceed 400 ° C, preferably 200 ° C. 15. Production of nanocomposite layers by thermal treatment of layers applied from solutions according to one or more of claims 1 to 7 and an electroactive polymer, wherein the nanostructures are produced directly in the applied layer consisting of nanostructure precursor compounds and electroactive polymer, and the temperature in the layer 400 ° C, preferably does not exceed 200 ° C. 16. Preparation of nanocomposite layers according to one or more of claims 9 and 15, wherein the nanostructures formed have sizes of less than 1 pm, preferably less than 100 nm. 17. Preparation of nanocomposite layers according to one or more of claims 9 and 16, wherein the layer thickness of these nanocomposite layers is less than 500 nm, preferably less than 250 nm. 18. Preparation of Nanocompositschichten according to one or more of claims 1 to 17, wherein as electroactive polymers, for example, polythiophenes, Polyfiuorene, polycarbazoles, polyphenylenes, Polyphenylenvinylene, polyanilines, polypyrroles, and / or derivatives thereof, oligomers and copolymers of these polymers are used. 19. Preparation of Nanocompositschichten according to one or more of claims 1 to 17, wherein instead of the electroactive polymer low molecular weight electroactive organic compounds, for example compounds and derivatives of these compounds from the families of phthalocyanines, perylenes, fullerenes, thiophenes, pentacenes, anthracenes, are used , JO • * * «« ♦ · * *** «► * · ft · · · ·« * • · «· · 20. Use of the nanocomposite layers according to one or more of claims 1 to 19 for the production of components or components such as solar cells, sensors or detectors, electrical or optical (including the UV, IR and microwave range) comprising components, switches, displays or radiation emitting Components such as lasers or light-emitting diodes (LEDs). 1. 5 2. 10 3. 15 4. 20 5. 6. 25 7. 30 8. 35 9. • • • * • * • · • * • · ♦ · • ·· ··· ♦. Changed claims: Preparation of a nanocomposite layer consisting of metal sulfide nanostructures and an electrically (haib) conductive polymer by applying a homogeneous solution of nanostructure precursor compounds and an electrically (semi) conductive polymer and subsequent direct conversion in the applied layer by energy input. Preparation of a nanocomposite layer consisting of metal sulfide nanostructures and an electrically (semi) conductive polymer, wherein a ternary, quaternary or more complex metal sulfide nanostructure is prepared by mixing different nanostructure precursor compounds according to claim 1, and the stoichiometry of the composition of this metal sulfide by the Mixture of the nanostructure precursor compound used is determined. Production of a nanocomposite layer according to claim 1 or 2, wherein the nanostructure precursor compounds are organic metal xanthates. Preparation of a nanocomposite layer according to claim 1 or 2, wherein the nanostructure precursor compounds are organic metal dithiocarbamates. Preparation of a nanocomposite layer according to claim 1 or 2, wherein the nanostructure precursor compounds represent organic metal trithiocarbonates. Preparation of a nanocomposite layer according to one of claims 1 to 5, wherein the energy input takes place by heat input at temperatures below 400 ° C, preferably below 200 ° C. Production of a nanocomposite layer according to one of Claims 1 to 5, the energy input being effected by energetic radiation, in particular by electron beams. Production of nanocomposite layers according to one of claims 1 to 7, wherein the nanostructures formed have sizes of less than 1 μην, preferably less than 100 nm. Production of nanocomposite layers according to one of claims 1 to 8, wherein the layer thickness of these nanocomposite layers is less than 500 nm, preferably less than 250 nm. POSSIBLE READY • I · I 4 «* * ·» · • I »« · · · · · «* · • I · * * · *» · * · • I · II ♦ · «· ·· -24- 10. Production of nanocomposite layers according to one of claims 1 to 9, wherein as electroactive polymers polythiophenes, polyfluorenes, polycarbazoles, polyphenylenes, polyphenylenevinylenes, polyanilines, polypyrroles, and / or their derivatives, oligomers 5 and copolymers of these polymers are used. 11. Preparation of Nanokompositschichten according to any one of claims 1 to 9, wherein instead of the electroactive polymer low molecular weight electroactive organic compounds from the group of phthalocyanines, perylenes, fullerenes, thiophenes, pentacenes, anthracenes are used. 12. Use of the nanocomposite layers according to one or more of claims 1 to 11 for the production of components or components, such as solar cells, sensors or detectors, electrical or optical (including the UV and IR and 15 microwave range) devices, switches, displays or radiation emitting components, such as lasers or light emitting diodes (LEDs). SUBSEQUENT