CN113500201B - Gold and preparation method and device of core-shell nanocrystalline thereof - Google Patents
Gold and preparation method and device of core-shell nanocrystalline thereof Download PDFInfo
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- CN113500201B CN113500201B CN202110737480.XA CN202110737480A CN113500201B CN 113500201 B CN113500201 B CN 113500201B CN 202110737480 A CN202110737480 A CN 202110737480A CN 113500201 B CN113500201 B CN 113500201B
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Abstract
The invention discloses a preparation method and a device of gold and core-shell nanocrystals thereof, wherein the preparation method comprises the following steps: mixing a reducing agent and a dispersing agent according to a certain volume ratio to prepare a reaction solution; adding chloroauric acid with preset mass into the reaction liquid; when the concentration of the chloroauric acid in the reaction liquid is a first mole number, generating zero-dimensional gold nanoparticles; when the concentration of the chloroauric acid in the reaction liquid is a second mole number, generating one-dimensional ultra-long gold nanowires; and when the concentration of the chloroauric acid in the reaction liquid is a third mole number, generating the two-dimensional gold nanosheets. The invention can control the morphology of the generated nanocrystalline by changing the concentration of chloroauric acid in the reaction liquid, has simple and convenient operation, and has very flexible control on the morphology of the nanocrystalline and is easy to repeat.
Description
Technical Field
The invention relates to the technical field of noble metal solution chemical synthesis, in particular to a preparation method and a device of gold and core-shell nanocrystals thereof.
Background
High quality nanocrystals are of great interest to researchers due to their unique optical, electronic, magnetic, etc. properties. Gold nano has potential application prospect in the fields of energy chemistry, biomedicine, food science and the like due to the unique size effect, surface effect, high potential and other properties. Therefore, the preparation of gold nanocrystals with different sizes and morphologies has important research significance.
The method for synthesizing the gold nanocrystals by a solution chemistry method comprises the following steps: white phosphorus reduction, sodium borohydride reduction, ethanol ultrasonic reduction, amine reduction, and the like. Among the above-mentioned techniques, basically used reducing agents include sodium borohydride, sodium citrate, oleylamine, ascorbic acid, tert-butylamine-borane complex, polyvinylpyrrolidone, and the like. Long amine reducing agents are of great interest in comparison to the strong reducing agent sodium borohydride reduction process due to their long-term stability in polar solvents. Sun et al first synthesized ultrafine, uniform, monodisperse gold nanocrystals in a tri-aqueous chloroauric acid, oleylamine, tetrahydronaphthalene, and tert-butylamine-borane complex system injection (Nano Res, 2008, 1, 229-234.). Zhang et al first placed oleylamine and trichlorfon in a vial and left to stand for 17 hours to obtain different types of gold nanocrystals and alloys derived from gold nanowires (nat. Chem., 2018, 4, 755-4330). In addition, gold palladium has great application value in the field of homogeneous catalysis, and the Xiao et al obviously improves the activation of the C-H bond of methane through limited-domain gold palladium nanocrystalline in a molecular sieve, thereby promoting the improvement of the yield of the methanol (Science, 2020, 367, 193-197). However, although researchers control and synthesize gold nanocrystals with different morphologies through various solution chemistry methods to serve scientific experimental researches corresponding to the researchers, currently, control and synthesize various required gold nanocrystals still has challenges, and various technical problems of unclear formation mechanism and action mechanism of different morphologies, poor repeatability and the like exist.
At present, the synthesis method of the synthesized gold nanocrystals is mainly focused on a seed crystal two-step growth method, namely, firstly synthesizing small-size gold nanocrystals, centrifuging and cleaning, taking gold nanocrystals as seed crystals, continuously feeding precursor chloroauric acid, reducing agent sodium borohydride, protecting agent cetyl trimethyl ammonium bromide and the like, and continuously growing nanocrystals with different morphologies. However, the two-step crystal growth method cannot flexibly control the morphology of the produced nanocrystals.
Disclosure of Invention
The invention provides a preparation method and a device of gold and core-shell nanocrystals thereof, which are used for overcoming at least one technical problem in the prior art.
According to a first aspect of an embodiment of the present invention, there is provided a method for preparing gold and core-shell nanocrystals thereof, including: mixing a reducing agent and a dispersing agent according to a certain volume ratio to prepare a reaction solution; adding chloroauric acid with preset mass into the reaction liquid; when the concentration of the chloroauric acid in the reaction liquid is a first mole number, generating zero-dimensional gold nanoparticles; when the concentration of the chloroauric acid in the reaction liquid is a second mole number, generating one-dimensional ultra-long gold nanowires; and when the concentration of the chloroauric acid in the reaction liquid is a third mole number, generating the two-dimensional gold nanosheets.
Optionally, after the step of generating the zero-dimensional gold nanoparticles, the method further comprises: and (3) increasing the reaction pressure to generate the one-dimensional short gold nanorods.
Optionally, after the step of generating the one-dimensional ultra-long gold nanowires, the method further comprises: and (3) growing palladium nanocrystals by epitaxy to generate gold-palladium core-shell structured nanowires.
Optionally, the decomposer comprises: 1, 2 dichloropropane or hexane, tetrahydronaphthalene; the reducing agent comprises: at least one of long chain amine or oleylamine, ascorbic acid, tert-butylamine-borane complex.
Optionally, the reaction solution is prepared as the raw materials; the volume ratio of the reducing agent to the dispersing agent in the reaction liquid is 1-4:0.1-1, the reaction temperature is 0-70 ℃, and the reaction time is 1-24 h.
According to a second aspect of the embodiment of the present invention, there is provided a preparation apparatus for gold and core-shell nanocrystals thereof, including: the configuration module is used for mixing the reducing agent and the dispersing agent according to a certain volume ratio to prepare a reaction solution; the adding module is used for adding chloroauric acid with preset mass into the reaction liquid; the first generation module is used for generating zero-dimensional gold nanoparticles when the concentration of the chloroauric acid in the reaction liquid is a first mole number; the second generation module is used for generating one-dimensional ultra-long gold nano wires when the concentration of the chloroauric acid in the reaction liquid is a second mole number; and the third generation module is used for generating the two-dimensional gold nano-sheet when the concentration of the chloroauric acid in the reaction liquid is a third mole number.
Optionally, the apparatus further includes: and the fourth generation module is used for increasing the reaction pressure and generating the one-dimensional short gold nanorods.
Optionally, the apparatus further includes: and the fifth generation module is used for generating gold-palladium core-shell structure nanowires through epitaxial growth of palladium nanocrystals.
Optionally, the decomposer comprises: 1, 2 dichloropropane or hexane, tetrahydronaphthalene; the reducing agent comprises: at least one of long chain amine or oleylamine, ascorbic acid, tert-butylamine-borane complex.
Optionally, the reaction solution is prepared as the raw materials; the volume ratio of the reducing agent to the dispersing agent in the reaction liquid is 1-4:0.1-1, the reaction temperature is 0-70 ℃, and the reaction time is 1-24 h.
The innovation points of the embodiment of the invention include:
1. according to the gold and the core-shell nanocrystalline method and device thereof, the gold with different qualities can be fixed through presetting and placed into the reaction liquid, so that the concentration of the gold in the reaction liquid is changed, the morphology of the produced nanocrystalline is further controlled, the operation is simple and convenient, and the control of the morphology of the produced nanocrystalline is very flexible and easy to repeat. Is one of the innovative points of the embodiments of the present invention.
2. The invention can synthesize a series of gold nanocrystals with different morphologies by a one-step method, has the characteristics of simple operation, high yield, easy repeatability, systematicness and the like, and has potential application prospects in the fields of photoelectrocatalysis, homogeneous catalysis and the like. Is one of the innovative points of the embodiments of the present invention.
3. The preparation method and the device of the gold-palladium core-shell nanocrystalline provided by the invention can be used for constructing novel noble metal nano building blocks based on gold nanocrystals with various morphologies, and the advantages of noble metals are complemented to achieve the maximum synergistic effect. Is one of the innovative points of the embodiments of the present invention.
4. The invention prepares a series of high-quality gold and core-shell nano-crystals thereof, and provides various options in terms of systemicity and target diversity. Is one of the innovative points of the embodiments of the present invention.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1a is a flow chart showing the steps of a method for preparing gold and core-shell nanocrystals according to the present invention;
FIG. 1b is a TEM image of 5 nm gold nanoparticles obtained in example 1;
FIG. 2 is a TEM image of 17 nm gold nanoparticles obtained in example 2;
FIG. 3 is a TEM image of 11 nm gold nanorods obtained in example 3;
FIG. 4 is a TEM image of the ultra-fine gold nanowires obtained in example 4;
FIG. 5 is a TEM image of the ultra-long gold nanowires obtained in example 5;
FIG. 6 is a TEM image of the gold nano-sheet obtained in example 6;
FIG. 7 is a TEM image of the ultra-long gold-palladium core-shell nanowire obtained in example 7;
fig. 8 is a schematic structural diagram of a device for preparing gold and core-shell nanocrystals thereof according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
It should be noted that the terms "comprising" and "having" and any variations thereof in the embodiments of the present invention and the accompanying drawings are intended to cover non-exclusive inclusions. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not limited to only those listed steps or elements but may include other steps or elements not listed or inherent to such process, method, article, or apparatus.
The embodiment of the invention discloses a preparation method and a device of gold and core-shell nanocrystalline. The following will describe in detail.
The invention provides a preparation method of gold and core-shell nanocrystals thereof, which can flexibly prepare gold nanoparticles, gold nanorods, gold nanowires and gold nanoparticles by adjusting the concentration of chloroauric acid. Referring to fig. 1a, fig. 1a is a schematic process flow diagram of a method for preparing gold and core-shell nanocrystals thereof according to the present invention. As shown in fig. 1a, the preparation method of gold and core-shell nanocrystals thereof comprises the following steps:
step 101, mixing a reducing agent and a dispersing agent according to a certain volume ratio to prepare a reaction solution.
Wherein the dispersant comprises 1, 2 dichloropropane or hexane, tetralin; the reducing agent comprises at least one of long chain amine or oleylamine, ascorbic acid, tert-butylamine-borane complex.
The reaction liquid is prepared at present, the volume ratio of the reducing agent to the dispersing agent in the reaction liquid is 1-4:0.1-1, the reaction temperature is 0-70 ℃, and the reaction time is 1-24 h.
In one implementation, the dispersant may further include at least one of chloroform, ethanol, deionized water, and acetone.
Step 102, adding chloroauric acid with preset mass into the reaction liquid.
In the step, chloroauric acid solid with preset mass can be added into the reaction liquid generated in the step 1, and nanocrystalline with different morphologies can be generated according to the concentration of the chloroauric acid in the reaction liquid after melting. The nanocrystals with different morphologies comprise gold nanoparticles, gold nanorods, gold nanowires and gold nanoparticles.
And 103, generating zero-dimensional gold nanoparticles when the concentration of chloroauric acid in the reaction solution is a first mole number.
In the step, when the concentration of chloroauric acid in the reaction solution is the first mole number, zero-dimensional gold nanoparticles are generated, and the size of the zero-dimensional gold nanoparticles is usually 5-20 nm.
The first mole number is 0.1 to 1 mmol; and adding chloroauric acid solid with preset mass into the reaction solution, wherein the concentration of the obtained chloroauric acid is a first mole number.
It is also noted that specific description of the generation of gold nanoparticles can be made with reference to examples 1 and 2.
Alternatively, when the dispersant is hexane and the concentration of chloroauric acid is a first mole number, one-dimensional ultrafine gold nanowires can be generated.
It should be further noted that, for a specific description of the generation of the one-dimensional ultrafine gold nanowires, reference may be made to example 4.
In one implementation, after step 104, the reaction pressure is increased to produce one-dimensional short gold nanorods.
Specific description of the formation of one-dimensional short gold nanorods can be given with reference to example 3.
And 104, generating the one-dimensional ultra-long gold nano-wire when the concentration of chloroauric acid in the reaction liquid is a second mole number.
In this step, when the concentration of chloroauric acid in the reaction solution is the second mole number, one-dimensional ultra-long gold nanowires are generated, and the length of the generated gold nanowires is typically 1 to 15 μm.
The second mole number includes less than 0.07 mmol; and adding chloroauric acid solid with preset mass into the reaction solution, wherein the concentration of the obtained chloroauric acid is a second mole number.
It should be further noted that, specific description of the generation of the one-dimensional ultra-long gold nanowire may refer to example 5.
In one implementation, after step 104, gold-palladium core-shell nanowires are generated by epitaxially growing palladium nanocrystals.
It should be noted that, all kinds of gold nanocrystals can be epitaxially grown with palladium on their surfaces to form a gold palladium core-shell structure; the core-shell structure also comprises gold platinum, gold palladium platinum, gold iridium, jin Lao, gold and silver, jin Liao.
It should be further noted that, for a specific description of the formation of gold-palladium core-shell nanowires, reference may be made to example 7.
And 105, when the concentration of chloroauric acid in the reaction solution is a third mole number, generating the two-dimensional gold nano-sheet.
In the step, when the concentration of chloroauric acid in the reaction solution is the third mole number, two-dimensional gold nano-sheets are generated, wherein the length-diameter ratio of the gold nano-sheets is generally 1-5 mu m.
The third mole number is 0.08-0.09 mmol; and adding chloroauric acid solid with preset mass into the reaction solution, wherein the concentration of the obtained chloroauric acid is a third mole number.
It should be noted that, for a specific description of the generation of the two-dimensional gold nanosheets, reference may be made to example 6.
Therefore, the gold and the core-shell nanocrystalline method thereof can be fixed by presetting chloroauric acid with different qualities, and the chloroauric acid is put into the reaction liquid, so that the concentration of the chloroauric acid in the reaction liquid is changed, and the morphology of the produced nanocrystalline is controlled. Specifically, when the concentration of chloroauric acid in the reaction liquid is 0.1-1 mmol, generating zero-dimensional gold nanoparticles; when the concentration of chloroauric acid in the reaction solution is lower than 0.07mmol, generating one-dimensional ultra-long gold nano-wires; when the concentration of chloroauric acid in the reaction solution is 0.08-0.09 mmol, the two-dimensional gold nanosheets are generated. The method is simple and convenient to operate, and the control on the morphology of the generated nano-crystals is very flexible and easy to repeat.
The specific experimental conditions are as follows:
example 1:
and preparing the zero-dimensional 5 nm gold nanoparticles. Dissolving 0.5-5 mmol chloroauric acid in 10-50 mL oleylamine and 10-50 mL tetrahydronaphthalene, cooling to a required temperature, injecting oleylamine/tetrahydronaphthalene mixed solution containing tert-butylamine-borane complex, vortex shaking, reacting at 0-60 ℃ for 0.5-2 h, and performing centrifugal separation and acetone washing for multiple times to obtain the superfine 5 nm gold nanoparticles. As shown in fig. 1b, fig. 1b is a TEM image of 5 nm gold nanoparticles prepared in example 1.
Example 2:
and preparing the zero-dimensional 12 nm gold nanoparticles. Dissolving 0.5-2 mmol chloroauric acid in 1-5 mL oleylamine and 0.1-1.5 mL 1, 2 dichloropropane, raising the temperature to a required temperature, standing for reaction at 0-70 ℃ for 1-24 h, and performing centrifugal separation and acetone washing for multiple times to obtain 12 nm gold nanoparticles. As shown in fig. 2, fig. 2 is a TEM image of 17 nm gold nanoparticles obtained in example 2.
Example 3:
11 nm gold nano-rods are prepared. Dissolving 0.1-0.9 mmol chloroauric acid in 1-5 mL oleylamine and 0.1-1.5 mL 1, 2 dichloropropane, raising the reaction pressure to 0-70 ℃ and the reaction time to 1-24 h, and obtaining the 11 nm gold nanorod through repeated centrifugal separation and acetone washing. As shown in fig. 3, fig. 3 is a TEM image of the 11 nm gold nanorods obtained in example 3.
Example 4:
preparing the one-dimensional superfine gold nano-wires. Dissolving 0.1-1 mmol chloroauric acid in 1-5 mL oleylamine and 0.1-1.5 mL hexane, raising the temperature to a required temperature, standing for reaction at 0-70 ℃ for 1-24 h, and performing centrifugal separation and acetone washing for multiple times to obtain the superfine gold nanowire. As shown in FIG. 4, FIG. 4 is a TEM image of the ultrafine gold nanowires obtained in example 4.
Example 5:
preparing the one-dimensional ultra-long gold nanowire. Dissolving 0.001-0.07 mmol chloroauric acid in 1-5 mL oleylamine and 0.1-1.5 mL 1, 2 dichloropropane, raising the temperature to a required temperature, standing for reaction at 0-70 ℃ for 1-24 h, and performing centrifugal separation and acetone washing for multiple times to obtain the ultra-long gold nanowire. As shown in FIG. 5, FIG. 5 is a TEM image of the ultra-long gold nanowires obtained in example 5.
Example 6:
preparing the two-dimensional gold nano-sheet. Dissolving proper 0.08-0.09 mmol chloroauric acid in 1-5 mL oleylamine and 0.1-1.5 mL 1, 2 dichloropropane, raising the temperature to a required temperature, standing for reaction at 0-70 ℃ for 1-24 h, and performing centrifugal separation and acetone washing for multiple times to obtain the gold nanosheets. FIG. 6 is a TEM image of the gold nano-sheet obtained in example 6, as shown in FIG. 6.
In one implementation, the precursor may include sodium chloropalladate in addition to chloroauric acid to produce ultra-long Jin Bana wires. Specific description is given in example 7.
Example 7:
based on the embodiment 5, dispersing 1-20 mg gold nanowires in ethanol, introducing 0.01-0.5 mM ascorbic acid into a reduced sodium chloropalladate aqueous solution under vortex vibration, and standing for 1-24 hours. And obtaining the ultra-long Jin Bana rice noodles through heart separation and acetone washing. As shown in fig. 7, fig. 7 is a TEM image of the ultra-long gold-palladium core-shell nanowire prepared in example 6.
In summary, the invention has the following advantages:
(1) The invention can synthesize a series of gold nanocrystals with different morphologies by a one-step method, has the characteristics of simple operation, high yield, easy repeatability, systematicness and the like, and has potential application prospects in the fields of photoelectrocatalysis, homogeneous catalysis and the like.
(2) The invention provides a preparation method of gold-palladium core-shell nanocrystals, which is based on gold nanocrystals with various shapes to construct novel noble metal nano building blocks, and the advantages of noble metals are complemented to achieve the maximum synergistic effect.
(3) The invention prepares a series of high-quality gold and core-shell nano-crystals thereof, and provides various options in terms of systemicity and target diversity.
The invention also provides a preparation device of the gold and the core-shell nanocrystalline thereof, and referring to fig. 8, fig. 8 is a schematic structural diagram of the preparation device of the gold and the core-shell nanocrystalline thereof. As shown in fig. 8, the preparation apparatus 80 of gold and core-shell nanocrystals thereof includes:
the configuration module 801 is configured to mix a reducing agent and a dispersing agent according to a certain volume ratio to prepare a reaction solution;
an adding module 802, configured to add chloroauric acid with a preset mass into the reaction solution;
a first generation module 803 for generating zero-dimensional gold nanoparticles when the concentration of the chloroauric acid in the reaction solution is a first mole number;
a second generating module 804, configured to generate a one-dimensional ultra-long gold nanowire when the concentration of the chloroauric acid in the reaction solution is a second mole number;
and a third generating module 805, configured to generate a two-dimensional gold nanosheet when the concentration of the chloroauric acid in the reaction solution is a third mole number.
Optionally, the apparatus further includes: and the fourth generation module is used for increasing the reaction pressure and generating the one-dimensional short gold nanorods.
Optionally, the apparatus further includes: and the fifth generation module is used for generating gold-palladium core-shell structure nanowires through epitaxial growth of palladium nanocrystals.
Optionally, the decomposer comprises: 1, 2 dichloropropane or hexane, tetrahydronaphthalene; the reducing agent comprises: at least one of long chain amine or oleylamine, ascorbic acid, tert-butylamine-borane complex.
Optionally, the reaction solution is prepared as the raw materials; the volume ratio of the reducing agent to the dispersing agent in the reaction liquid is 1-4:0.1-1, the reaction temperature is 0-70 ℃, and the reaction time is 1-24 h.
Therefore, the gold and the preparation device of the core-shell nanocrystalline thereof provided by the invention can be fixed by presetting chloroauric acid with different qualities, and can be put into a reaction solution to change the concentration of the chloroauric acid in the reaction solution, so that the morphology of the produced nanocrystalline is controlled. Specifically, when the concentration of chloroauric acid in the reaction liquid is 0.1-1 mmol, generating zero-dimensional gold nanoparticles; when the concentration of chloroauric acid in the reaction solution is lower than 0.07mmol, generating one-dimensional ultra-long gold nano-wires; when the concentration of chloroauric acid in the reaction solution is 0.08-0.09 mmol, the two-dimensional gold nanosheets are generated. The method is simple and convenient to operate, and the control on the morphology of the generated nano-crystals is very flexible and easy to repeat.
Those of ordinary skill in the art will appreciate that: the drawing is a schematic diagram of one embodiment and the modules or flows in the drawing are not necessarily required to practice the invention.
Those of ordinary skill in the art will appreciate that: the modules in the apparatus of the embodiments may be distributed in the apparatus of the embodiments according to the description of the embodiments, or may be located in one or more apparatuses different from the present embodiments with corresponding changes. The modules of the above embodiments may be combined into one module, or may be further split into a plurality of sub-modules.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (3)
1. The preparation method of gold and the core-shell nanocrystalline thereof is characterized by comprising the following steps:
mixing a reducing agent and a dispersing agent according to a certain volume ratio to prepare a reaction solution;
adding chloroauric acid with preset quality into the reaction liquid, and changing the concentration of the chloroauric acid in the reaction liquid by presetting chloroauric acids with different qualities so as to control the morphology of the generated nanocrystalline;
when the concentration of the chloroauric acid in the reaction liquid is a first mole number, generating zero-dimensional gold nanoparticles; wherein when the first mole number is 0.5-5 mmol, the adopted reducing agent is 10-50 mL oleylamine and the dispersing agent is 10-50 mL tetrahydronaphthalene; or when the first mole number is 0.5-2 mmol, the adopted reducing agent is 1-5 mL oleylamine and the dispersing agent is 0.1-1.5 mL 1, 2 dichloropropane;
when the concentration of the chloroauric acid in the reaction liquid is a second mole number, generating one-dimensional ultra-long gold nanowires; wherein when the second mole number is 0.001-0.07 mmol, the adopted reducing agent is 1-5 mL oleylamine and the dispersing agent is 0.1-1.5 mL 1, 2 dichloropropane; or when the second mole number is 0.1-1 mmol, the adopted reducing agent is 1-5 mL oleylamine and the dispersing agent is 0.1-1.5 mL hexane;
when the concentration of the chloroauric acid in the reaction liquid is a third mole number, generating a two-dimensional gold nano-sheet; wherein when the third mole number is 0.08-0.09 mmol, the adopted reducing agent is 1-5 mL oleylamine and the dispersing agent is 0.1-1.5 mL 1, 2 dichloropropane.
2. The method of claim 1, wherein after the step of generating one-dimensional ultra-long gold nanowires, the method further comprises:
and (3) growing palladium nanocrystals by epitaxy to generate gold-palladium core-shell structured nanowires.
3. The method of claim 1, wherein the step of determining the position of the substrate comprises,
the reaction liquid is prepared for use at present;
the reaction temperature of the reaction liquid is 0-70 ℃ and the reaction time is 1-24 h.
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