CN109988338B - Nano composite material and preparation method and application thereof - Google Patents
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- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
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Abstract
The invention relates to the technical field of quantum dot materials, and particularly provides a nano composite material and a preparation method and application thereof. The nano composite material comprises a ligand modified quantum dot and a compatibilizer coated on the surface of the ligand modified quantum dot, wherein the compatibilizer has a fatty acid carbon chain and an active functional group, and the fatty acid carbon chain is combined with the ligand. The preparation method comprises the following steps: and (3) coating the quantum dots modified by the ligands by using a compatibilizer, so that the compatibilizer and the ligands are subjected to self-assembly and are coated on the surfaces of the quantum dots modified by the ligands, and the quantum dots coated by the compatibilizer are obtained. According to the nano composite material, the compatibilizer is coated on the surface of the quantum dot modified by the ligand, so that the quantum dot has good dispersibility, the compatibility with other polymers is greatly improved, the quantum dot can be well dispersed in other high molecular compounds, and the obtained nano composite material has good transparency and high fluorescence intensity.
Description
Technical Field
The invention belongs to the technical field of quantum dot materials, and particularly relates to a nano composite material and a preparation method and application thereof.
Background
Quantum dots, also known as nanocrystals, are nanoparticles composed of group II-VI or group III-V elements. The particle diameter of the quantum dot is generally between 1 nm and 10nm, and as electrons and holes are limited by quanta, a continuous energy band structure is changed into a discrete energy level structure with molecular characteristics, and fluorescence can be emitted after stimulation. Based on quantum effect, the quantum dots have wide application prospect in the fields of solar cells, luminescent devices, optical biomarkers and the like.
The quantum dots have a very large specific surface area due to their small particle size, and the increase in the number of surface phase atoms results in insufficient coordination of surface atoms, an increase in unsaturated bonds and dangling bonds (i.e., unpaired electrons on the surface of the crystal lattice), and thus these surface atoms have high activity and are very unstable and easily bonded to other atoms. Therefore, the surface of the quantum dot generally needs to select a proper ligand to coordinate with the metal on the surface of the quantum dot, and the type of the ligand has a decisive influence on the efficiency and stability of the quantum dot. With the development and optimization of the quantum dot synthesis technology, the efficiency and stability of the quantum dots reach the industrialization level. However, the unique surface effect of the quantum dot also determines the sensitivity of the quantum dot to moisture and oxygen, which can destroy the ligand on the surface of the quantum dot and reduce the efficiency of the quantum dot. The smaller the size of the quantum dot, the larger the specific surface area, and the higher the sensitivity to moisture and oxygen.
Researches have found that the excitation spectrum of the semiconductor quantum dot/epoxy resin composite material is very wide and the luminous intensity is high, so that the epoxy resin has attracted much attention in recent years as a packaging material of white light LEDs. However, due to the surface effect and the mismatching of the interface, the quantum dots tend to agglomerate in the polar epoxy resin matrix, so that it is difficult to prepare the composite nano material with high transparency and high fluorescence intensity.
In the composite nano material, the matching degree of the two-phase interface polarity directly determines the dispersion state of the nano material in a matrix and the performance of the final nano composite material. However, due to the non-polar carbon chain structure on the surface of the quantum dot, the quantum dot itself cannot be directly and effectively dispersed in the polar epoxy resin, and the transparency of the nanocomposite material is reduced and the fluorescence intensity is weakened.
Disclosure of Invention
The invention aims to provide a composite nano material and a preparation method thereof, and aims to solve the problems of low transparency, weak fluorescence intensity and the like of an obtained nano composite material caused by poor mutual dispersibility and easy agglomeration of high-molecular compounds such as quantum dots, epoxy resin and the like in the prior art.
Further, the invention also provides application of the composite nano material.
The invention is realized by the following steps: a nanocomposite material comprises ligand-modified quantum dots and a compatibilizer coated on the surfaces of the ligand-modified quantum dots, wherein the compatibilizer has a fatty acid carbon chain and an active functional group, and the fatty acid carbon chain and the ligand are combined with each other.
Correspondingly, the preparation method of the nano composite material at least comprises the following steps:
and (3) coating the quantum dots modified by the ligands by using a compatibilizer, so that the compatibilizer and the ligands are subjected to self-assembly and are coated on the surfaces of the quantum dots modified by the ligands, and the quantum dots coated by the compatibilizer are obtained.
Accordingly, the application of the nanocomposite material or the nanocomposite material prepared by the preparation method of the nanocomposite material in the fields of solar cells, light emitting devices and optical biomarkers is provided.
The invention has the following beneficial effects: according to the nano composite material provided by the invention, the surface of the ligand-modified quantum dot is coated with the compatibilizer, so that the agglomeration effect of the quantum dot is reduced under the action of the compatibilizer, the quantum dot can be uniformly dispersed in high molecular compounds such as epoxy resin, and the obtained nano composite material shows good transparency and high fluorescence intensity.
According to the preparation method of the nano composite material, the compatibilizer is directly coated on the surface of the quantum dot modified by the ligand, so that the compatibility of the quantum dot and a high molecular compound is improved, the agglomeration phenomenon of the quantum dot is avoided, the quantum dot can be uniformly dispersed in the high molecular compound, and the nano composite material with high transparency and strong fluorescence intensity is finally obtained. Moreover, the preparation method of the nano composite material provided by the invention has the advantages of simple and easily-controlled process, low cost and easy realization of industrial production.
The nano composite material provided by the invention has the characteristics of good transparency, strong fluorescence emission and the like, and is very suitable for the fields of solar cells, luminescent devices, optical biomarkers and the like.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a nano composite material. The nano composite material comprises a ligand modified quantum dot and a compatibilizer coated on the surface of the ligand modified quantum dot, wherein the compatibilizer has a fatty acid carbon chain and an active functional group, and the fatty acid carbon chain is combined with the ligand.
The nano composite material disclosed by the invention has the advantages that the quantum dots and the surface are coated with the compatibilizer, and the agglomeration among the quantum dots is reduced or even avoided under the action of the compatibilizer and the ligand, so that the quantum dots are uniformly dispersed, and therefore, when the nano composite material is mixed with other high molecular compounds, the nano composite material shows high transparency and can emit strong fluorescence after being stimulated.
Further, the nanocomposite material also includes a polymer compound. The nano composite material containing the high molecular compound can effectively avoid the contact of the quantum dots with water, oxygen and the like, and greatly improves the efficiency of the quantum dots.
Preferably, the polymer compound is an epoxy resin.
In the invention, the structure formed by the quantum dots and the compatibilizer can be a core-shell structure or not, and the microstructure of the nanocomposite material of the invention is not limited thereby.
The quantum dots can be nanoparticles composed of II-VI or III-V elements, and the particle size of the nanoparticles is 1-10 nm.
Preferably, the quantum dot is any one of CdSe, CdS, CdTe, CdSe/ZnS, CdSn/ZnS, PbSe, PbS, PbSe/ZnS and PbSe/CdS. The quantum dots form a good ligand structure under the action of ligand oleic acid, and can greatly improve the compatibility of the quantum dots and other polar organic matters.
Preferably, the ligand used by the ligand-modified quantum dot is an organic substance containing carboxyl and a carbon chain, the carboxyl and the quantum dot form the ligand, and the carbon chain is suspended on the surface of the quantum dot, so that the compatibility of the quantum dot and other substances is improved.
Preferably, the organic matter containing carboxyl and carbon chain is fatty acid, the fatty acid has carboxyl and carbon chain, the carboxyl can form good ligand with the quantum dot, and the carbon chain modifies the surface of the quantum dot, so that the quantum dot has better compatibility with other organic matters. Of course, the fatty acid involved in the present invention may be a clathrate fatty acid or an unsaturated fatty acid.
More preferably, the fatty acid is oleic acid (also called cis-octadecene-9-oic acid), the oleic acid has a terminal carboxyl group and a nonpolar carbon chain structure, the terminal carboxyl group can form a good ligand structure with the quantum dot, and the nonpolar carbon chain modifies the surface of the quantum dot, so that the compatibility of the quantum dot and other polar organic matters is greatly improved.
The quantum dot is coated with the compatibilizer with the epoxy functional group, and the compatibilizer has the epoxy functional group, so that the compatibility of the compatibilizer and a high molecular compound material can be improved, the dispersion effect of the compatibilizer on the surface of the quantum dot and other high molecular compounds is better, and the agglomeration phenomenon of the quantum dot is avoided.
Preferably, the compatibilizer is an epoxy-functionalized fatty acid. Epoxy-functionalized fatty acids have, on the one hand, a functional group of an epoxy group and, on the other hand, a carbon chain of the fatty acid. When the epoxy resin is mixed with a quantum dot which takes fatty acid as a ligand, the carbon chain on the surface of the quantum dot and the carbon chain of the compatibilizer are subjected to self-assembly, and the epoxy group forms a layer of structure which surrounds the surface of the quantum dot and faces outwards.
Still more preferably, the compatibilizer is an epoxy functional group-modified oleic acid. When the compatibilizer is epoxy functionalized oleic acid and the ligand of the quantum dot is oleic acid, and the compatibilizer and the ligand-modified quantum dot are mixed, carbon chains on the compatibilizer and carbon chains on the ligand are automatically aggregated and mutually organized into a regular structure, so that the compatibilizer and the quantum dot are combined into a nano structure with ordered arrangement, and epoxy groups on the epoxy functionalized oleic acid are consistent and outward, so that the quantum dot can be well and uniformly dispersed in other high molecular compounds, such as epoxy resin.
Preferably, the polymer compound is an epoxy resin.
The nano composite material of the invention effectively improves the surface effect and the interface matching property of the quantum dots on the basis of the structure and the composition, and the quantum dots are uniformly distributed in the high molecular compound, so that the nano composite material shows the characteristics of high transparency and high fluorescence intensity.
Correspondingly, the invention further provides a preparation method of the nanocomposite material on the basis of providing the nanocomposite material. That is, the nanocomposite material of the above structure can be produced by the present production method.
In one embodiment, the method for preparing the nanocomposite at least comprises the following steps:
s01, adopting a compatibilizer to coat the quantum dots modified by the ligand,
and enabling the compatibilizer and the ligand to perform self-assembly and cover the surface of the quantum dot modified by the ligand, so as to obtain the quantum dot covered by the compatibilizer.
The technical solution of the present invention is explained in detail below.
In any embodiment, the ligand-modified quantum dot refers to a quantum dot that is subjected to a mixing treatment with a ligand before a coating treatment with a compatibilizer, so that the quantum dot is coordinated with the ligand to form a complex.
Preferably, the quantum dot is any one of CdSe, CdS, CdTe, CdSe/ZnS, CdSn/ZnS, PbSe, PbS, PbSe/ZnS and PbSe/CdS.
The compatibilizer can be the existing compatibilizer with epoxy functional groups and can also be prepared by self. Taking as an example a compatibilizer with epoxy functionality such as epoxy-functional modified oleic acid, can be formulated as follows:
mixing epoxy resin and oleic acid according to the weight ratio of (1-4) g: (1-6) mL, and heating the mixture to prepare the epoxy functionalized oleic acid.
In the specific preparation, in order to ensure the balance of the reaction temperature, the carboxyl group on the oleic acid can react with the epoxy in an oil bath environment, for example, in an oil bath at the temperature of 100-200 ℃ for 3-24h, so that the epoxy functional group modified oleic acid can be obtained.
Preferably, in step S01, the charging ratio of the quantum dot to the compatibilizer is (1-4): (2-8), under the mixture ratio, the compatibilizer is fully modified on the surface of the quantum dot, so that the quantum dot is prevented from being not completely coated, and meanwhile, the coating layer of the compatibilizer is prevented from being too thick.
In the process of coating the compatibilizer and the quantum dots, ultrasonic treatment can be carried out for 20-60min, the ultrasonic frequency only needs to be treated according to conventional ultrasonic equipment, and the epoxy functionalized quantum dots can be obtained by centrifugal treatment after the ultrasonic treatment. In order to improve the coating effect, the compatibilizer can be dissolved in the solvent, for example, the compatibilizer can be dissolved in tetrahydrofuran to form a tetrahydrofuran solution with the compatibilizer concentration of 5-20 wt%. After coating, the solvent can be removed by heating, and the quantum dots coated by the compatibilizer can also be left in the solvent for further coating treatment.
When oleic acid modified by epoxy functional groups is used as a compatibilizer and quantum dots taking the oleic acid as a ligand are coated, the carbon chains on the compatibilizer and the carbon chains of the quantum dot ligand are subjected to self-assembly to form a uniform and ordered self-assembly structure on the surface of the quantum dots, at the moment, the compatibilizer is attached to the surface of the quantum dots, and the epoxy functional groups on the compatibilizer face outwards, so that a good microscopic surface is provided for good dispersion compatibility with materials such as other high molecular compounds.
After the quantum dot coated with the compatibilizer obtained in the step S01 is processed, the method further includes mixing and curing the high molecular compound and the quantum dot coated with the compatibilizer.
When a high molecular compound and the quantum dots coated by the compatibilizer are mixed, the feeding proportion of the quantum dots to the high molecular compound is (1-2): (1-3).
In the process of mixing the quantum dots and the high molecular compound, the quantum dots coated with the compatibilizer can be directly mixed with the high molecular compound, or the quantum dots coated with the compatibilizer can be dissolved in a solvent to form a tetrahydrofuran solution with the quantum dot concentration of about 1-5 wt%, and then the tetrahydrofuran solution and the high molecular compound are mixed to be uniform.
Preferably, the polymer compound is an epoxy resin. The epoxy resin is adopted mainly because the epoxy resin has good compatibility with an epoxy functional group on the compatibilizer, so that the dispersibility of the quantum dots is greatly improved. Needless to say, the polymer compound of the present invention is not limited to the epoxy resin, and may be polymethyl methacrylate (PMMA) or the like.
The curing treatment refers to a curing treatment of a product obtained by mixing the quantum dots coated with the compatibilizer and the polymer compound with a curing agent, and mainly cures the polymer compound. By curing, the polymer compound is crosslinked into a polymer material having stable chemical properties.
Preferably, the curing agent is any one of a phenol-aldehyde amine curing agent, an acid anhydride curing agent, an imidazole curing agent and a thiol curing agent. The curing agent of the present invention should be compatible with the polymer compound when used, and the polymer compound, the curing agent and the curing process are all known in the art, and the material ratio is common knowledge, so the polymer compound, the curing agent and the curing process are not described in detail in the present invention.
Before the curing treatment, it is necessary to remove the solvent by heating, so as to avoid the occurrence of voids due to the presence of the solvent. Before curing, it is necessary to heat to remove bubbles and remove gas in the mixture of the high molecular compound and the quantum dots, so as to achieve better effect of avoiding generation of blisters.
During curing, the nano composite material can be subjected to die filling according to different requirements, and curing treatment is carried out in a die, so that the nano composite materials of different models are finally obtained.
According to the preparation method of the nano composite material provided by the embodiment of the invention, the compatibilizer is directly coated on the surface of the quantum dot modified by the ligand, and then the quantum dot and the high molecular compound are mixed and cured, so that the compatibility of the quantum dot and the high molecular compound is improved, the agglomeration phenomenon of the quantum dot is avoided, the quantum dot is uniformly dispersed in the high molecular compound, and the nano composite material with high transparency and strong fluorescence intensity is finally obtained. Moreover, the preparation method of the nano composite material provided by the invention has the advantages of simple and easily-controlled process, low cost and easy realization of industrial production.
For example, in the quantum dot using oleic acid as a ligand, since oleic acid can be adsorbed to the surface of the quantum dot through the coordination of carboxyl and a hollow orbit on the surface of the quantum dot, and the carbon chain structure of oleic acid is outward, a layer of wrapped nonpolar structure is formed on the surface of the quantum dot, when the quantum dot is coated by the compatibilizer, an aliphatic side chain of the compatibilizer and the carbon chain of oleic acid are self-assembled on the surface of the quantum dot, and an epoxy group at the other end of the compatibilizer is outward, so that the quantum dot modified by the compatibilizer has similar polarity to that of an epoxy matrix, and when epoxy resin is used as a high molecular compound, a good interface compatibility effect can be achieved.
In general, the interface effect and the interface matching property of the nano composite material prepared by the embodiment of the invention are greatly improved, the contact with water and oxygen is avoided, and the nano composite material has the characteristics of high transparency, high fluorescence intensity and the like. Therefore, the method can be applied to the fields of solar energy, luminescent devices, optical biomarkers and the like.
In order to better explain the technical solution of the present invention, the following description is made with reference to specific examples.
Example 1
A method for preparing a nanocomposite, the process for preparing the nanocomposite comprising the steps of:
s11, preparing a compatibilizer: weighing 5g of epoxy resin (E51) and 5mL of oleic acid, placing the obtained epoxy resin and the oleic acid in a single-neck round-bottom flask together, and reacting for 3 hours in an oil bath at 100 ℃ to obtain a compatibilizer with an epoxy functional group;
s12, preparing the quantum dot modified by the compatibilizer: dissolving a ligand (containing 5g of CdSe quantum dots) formed by oleic acid and CdSe quantum dots and 10g of the compatibilizer obtained in the step S11 in tetrahydrofuran, performing ultrasonic treatment for 20min, and then centrifuging the mixture in a centrifuge at the rotating speed of 3000rpm for 3min to obtain epoxy group functionalized quantum dots, so that the compatibilizer is coated on the surfaces of the quantum dots;
s13, mixing 2g of the quantum dots coated with the compatibilizer obtained in the step S12 with tetrahydrofuran to form a solution, adding 2g of epoxy resin (E51) into the solution, stirring the solution at room temperature until the solution is uniform, then drying the solution in a vacuum drying oven at 40 ℃ for 1 hour, removing a tetrahydrofuran solvent, taking the solution out after cooling, adding about 0.25g of triethylene tetramine into the solution, stirring the solution uniformly at 40 ℃ while removing bubbles in the mixed material, and then curing the solution in the drying oven at 60 ℃ for 2 hours to obtain the nanocomposite combining the quantum dots and the epoxy resin.
Example 2
A method for preparing a nanocomposite, the process for preparing the nanocomposite comprising the steps of:
s21, preparing a compatibilizer: weighing 20g of epoxy resin (AG-80) and 30mL of oleic acid, placing the obtained epoxy resin and the oleic acid into a single-neck round-bottom flask together, and reacting for 24 hours in an oil bath at 200 ℃ to obtain a compatibilizer with an epoxy functional group;
s22, preparing the quantum dot modified by the compatibilizer: dissolving a ligand (containing 20g of CdSe quantum dots) formed by oleic acid and CdSe quantum dots and 20g of the compatibilizer obtained in the step S21 in tetrahydrofuran, performing ultrasonic treatment for 60min, and then centrifuging the mixture in a centrifuge at the rotating speed of 8000rpm for 10min to obtain epoxy group functionalized quantum dots so as to realize the coating of the compatibilizer on the surfaces of the quantum dots;
s23, adding 5g of the quantum dots coated with the compatibilizer obtained in the step S22 into tetrahydrofuran to form a solution, adding 5g of epoxy resin (AG-80) into the solution, stirring the solution at room temperature until the solution is uniform, then drying the solution in a vacuum drying oven at 80 ℃ for 3h, removing a tetrahydrofuran solvent, taking out the solution after cooling, adding about 0.85g of triethylene tetramine into the solution, stirring the solution uniformly at 60 ℃ while removing bubbles in the mixed material, and then curing the solution in the drying oven at 90 ℃ for 6h to obtain the nanocomposite combining the quantum dots and the epoxy resin.
Comparative example 1
A method for preparing a nanocomposite, the process for preparing the nanocomposite comprising the steps of:
D11. dissolving 5g of CdSe quantum dots in tetrahydrofuran, adding 5g of epoxy resin (E51) into the CdSe quantum dots, stirring the mixture at room temperature until the mixture is uniform, then putting the mixture into a vacuum drying oven at 40 ℃ for drying for 1h, removing the tetrahydrofuran solvent, taking the mixture out after cooling, adding about 0.55g of triethylene tetramine into the mixture, stirring the mixture uniformly at 40 ℃ while removing bubbles in the mixture, and then curing the mixture in an oven at 60 ℃ for 2h to obtain the nanocomposite with the quantum dots combined with the epoxy resin.
In order to illustrate the technical effects of the nanocomposite material of the present invention, the nanocomposite materials obtained in examples 1-2 and comparative example 1 were subjected to test analysis of the transparency and fluorescence characteristics.
The specific implementation method of the transparent characteristic is as follows:
the transparency of the obtained nanocomposites was characterized by using model 3500 (Shimadzu corporation, Japan) UV-visible spectrophotometer, which was conducted in a transmission mode with air as a background, each material was tested 5 times, and the average value was averaged and recorded in Table 1.
Second, fluorescent characteristic test
The obtained nanocomposites were characterized for their fluorescence properties using a fluorescence spectrophotometer model F4500 (hitachi, japan), each material was tested 5 times, averaged, and the test average was recorded in table 1.
TABLE 1 nanocomposite Performance test results of examples 1-2 and comparative example 1
Group of | Example 1 | Example 2 | Comparative example 1 |
Average value of visible light transmittance at 800nm | 76% | 81% | 43% |
Average value of fluorescence intensity at 550nm | 1682000 | 1750027 | 607108 |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (12)
1. A nanocomposite material is characterized by comprising ligand-modified quantum dots and a compatibilizer coated on the surfaces of the ligand-modified quantum dots, wherein the compatibilizer has a fatty acid carbon chain and an active functional group, and the fatty acid carbon chain and the ligand are combined with each other;
wherein the compatibilizer is oleic acid modified by epoxy functional groups.
2. The nanocomposite of claim 1, wherein the reactive functional group is an epoxy functional group.
3. The nanocomposite of claim 1, wherein the ligand is oleic acid; and/or the quantum dots are any one of CdSe, CdS, CdTe, CdSe/ZnS, CdSn/ZnS, PbSe, PbS, PbSe/ZnS and PbSe/CdS.
4. Nanocomposite material according to any one of claims 1 to 3, wherein the nanocomposite material further comprises a macromolecular compound.
5. Nanocomposite as claimed in claim 4, characterized in that the macromolecular compound is an epoxy resin.
6. A method for preparing a nanocomposite, characterized by at least comprising the steps of:
adopting a compatibilizer to coat the quantum dots modified by the ligand, so that the compatibilizer and the ligand are subjected to self-assembly and coat the surfaces of the quantum dots modified by the ligand to obtain the quantum dots coated by the compatibilizer; wherein the compatibilizer has a fatty acid carbon chain and an active functional group, the fatty acid carbon chain and the ligand are bonded to each other;
wherein the compatibilizer is oleic acid modified by epoxy functional groups.
7. The method of claim 6, wherein the step of obtaining the compatibilizer coated quantum dot further comprises: and mixing and curing the high molecular compound and the quantum dots coated by the compatibilizer.
8. The method for preparing the nanocomposite material as claimed in claim 6, wherein the charging ratio of the quantum dots to the compatibilizer is (1-4): (2-8).
9. The method of claim 6, wherein the reactive functional group is an epoxy functional group.
10. The method of preparing a nanocomposite as claimed in any of claims 6 or 7, wherein the ligand is oleic acid; and/or the quantum dots are any one of CdSe, CdS, CdTe, CdSe/ZnS, CdSn/ZnS, PbSe, PbS, PbSe/ZnS and PbSe/CdS.
11. The method of claim 7, wherein the polymer compound is an epoxy resin.
12. Use of a nanocomposite material according to any one of claims 1 to 5 or a nanocomposite material prepared by a method for preparing a nanocomposite material according to any one of claims 6 to 11 in the field of solar cells, light emitting devices, optical biomarkers.
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