CN108941611B - Preparation method and product of ferromagnetic nanowire - Google Patents
Preparation method and product of ferromagnetic nanowire Download PDFInfo
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Abstract
The invention relates to a preparation method of ferromagnetic nano-wire and its product, belonging to the technical field of nano-material, firstly using ferromagnetic metal salt, stabilizing agent, complexing agent and surfactant as raw material to prepare ferromagnetic metal salt mixed solution, then injecting reducing agent solution by means of injection, after reaction to obtain solid product, cleaning and drying said solid product so as to obtain the invented product. The method has the advantages of simple synthetic route, controllable process, normal temperature and pressure reaction, accordance with the actual production requirement, suitability for industrial production, and capability of overcoming the defect that the traditional in-situ reduction method can only prepare the ferromagnetic nanowire with a certain length-diameter ratio. The ferromagnetic nanowire prepared by the method has good orientation, the diameter is less than 100nm, the length is 3-10 mu m, the length-diameter ratio is high, and the ferromagnetic nanowire has good flexibility, magnetic performance and microwave absorption performance.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a ferromagnetic nanowire and a product.
Background
The ferromagnetic nanowires are of the nanoscale (E)-9m) iron atoms are stacked and grown according to a certain direction to form the one-dimensional nano material. The nanometer size and the unique structure enable the ferromagnetic nanowire to show unique physical effects which many bulk phase materials do not have, mainly including small size effect, surface interface effect, quantum size effect, macroscopic quantum tunneling effect and the like. The unique structure and peculiar optical, electric, magnetic and other properties make the ferromagnetic nano-wire increasingly widely used in various fields of social industry. For example, a large saturation magnetization, a high coercivity, good oxidation resistance, a high signal-to-noise ratio, such thatThe high-performance magnetic recording material based on the ferromagnetic nanowires can greatly improve the performance of a magnetic tape and a large-capacity soft and hard magnetic disk; the ferromagnetic nanowire has a wave absorbing mechanism different from that of a conventional material, shows excellent absorption performance on electromagnetic waves in a wide frequency band range, and is widely applied to composite and structural stealth materials such as electromagnetic wave stealth materials, visible light-infrared light stealth materials and the like in a microwave frequency band in military, and electromagnetic radiation shielding materials; the guiding agent based on the ferromagnetic nanowire as the carrier can utilize the soft magnetic characteristic of the ferromagnetic nanowire to gather high-concentration drugs at a focus part under the action of an external magnetic field, so that targeted therapy is performed on pathological parts; the ferrofluid taking the ferromagnetic nanowires as magnetic particles has good anti-settling property and shear yield stress, and shows great application potential in the fields of vibration reduction, sealing, polishing, sound adjustment, medical appliances, optical display and the like; in addition, ferromagnetic nanowires are also widely used as catalysts for growth of silicon nanowires and carbon nanofibers. The excellent performance and wide application of ferromagnetic nanowires have made them one of the research hotspots in material science and condensed state physics.
Template synthesis, lithography and metal evaporation are three common methods for preparing ferromagnetic nanowires. The ferromagnetic nano-wire is prepared by a template method, wherein the generated ferromagnetic particles are self-assembled along the aperture to form the nano-wire by reaction in a film with a nano-scale aperture, and then the film serving as the template is removed by using a strong corrosive agent, so that the purity of the ferromagnetic nano-wire is inevitably affected and the environment is also harmed to a certain extent; the lithography technology utilizes an external directional magnetic field to self-assemble ferromagnetic particles on a substrate into regular nanowires, the process relates to the selection of parameters of the substrate and the magnetic field, and the yield is low, so that the preparation cost is higher; for example, chinese patent No. cn200410088423.x discloses a method for growing a single-crystal iron nanowire on a silicon substrate by connecting a spiral iron wire to an electrode and heating the wire by applying a current of 20 to 35 amperes, so that the evaporated iron wire is deposited on the silicon substrate, and there is a phenomenon that a nanowire is formed by solidifying ferromagnetic particles formed by evaporating ferromagnetic metal particles or wires at a high temperature on the substrateComplex operation, low yield, high cost and the like. To overcome the above-mentioned disadvantages, some new methods for preparing ferromagnetic nanowires have emerged, and chinese patent CN200710056737.5 discloses a method for preparing ferromagnetic nanowires, which comprises adding sodium hydroxide or ammonia water into ferric nitrate solution to obtain fe (oh)3Then mixing with sodium chloride according to a certain mass ratio and ball-milling to obtain Fe (OH)3And (3) after the/NaCl composite powder is subjected to reduction by using hydrogen at a certain temperature to obtain Fe/NaCl, and finally, the Fe nanowire is obtained by ultrasonic cleaning of deionized water. The method has complex operation steps and relates to professional equipment with high requirements on ball milling, hydrogen reduction and the like. Chinese patent CN200610018655.7 and Wanquan Jiang et al (Jiang W Q et al, J.Magn.Magn.Mater., 323(2011) 3246) of the university of Chinese science and technology) use an in-situ reduction method to dissolve soluble ferrous iron or ferric iron salt as a raw material in distilled water to prepare an iron salt solution, and dropwise add a reducing agent solution into the iron salt solution to react, filter and dry to prepare the iron nanowire. The whole process is carried out at normal temperature, the synthetic route is simple, however, the dripping process is slow, and the length-diameter ratio of the prepared iron nanowire is limited.
Therefore, a preparation method which has simple process and high speed and ensures that the finally prepared ferromagnetic nanowire has high purity, good dispersibility, uniform size and controllable length is urgently needed.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing ferromagnetic nanowires; the second purpose is to provide a ferromagnetic nanowire.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a method of preparing ferromagnetic nanowires, the method comprising the steps of:
(1) dissolving ferromagnetic metal salt in water, then adjusting the pH value to 10-12, adding a stabilizer, a complexing agent and a surfactant, stirring, and removing oxygen in the solution to form a ferromagnetic metal salt mixed solution; the concentration of the ferromagnetic metal salt in the ferromagnetic metal salt mixed solution is 0.05-0.15 mol/L, the concentration of the stabilizer is 0.02-0.04 mol/L, the concentration of the complexing agent is 0.001-0.002 mol/L, and the concentration of the surfactant is 0.002-0.003 mol/L;
(2) dissolving a reducing agent in the solution to form a reducing agent solution; the concentration of the reducing agent in the reducing agent solution is 0.9-2 mol/L;
(3) and (3) introducing the reducing agent solution formed in the step (2) into the ferromagnetic metal salt mixed solution formed in the step (1) in an injection mode, reacting for 30-45 min at 20-40 ℃ after the reducing agent solution is injected, obtaining a solid product, and cleaning and drying the solid product.
Preferably, in the step (1), the ferromagnetic metal salt is one of iron salt, nickel salt or cobalt salt.
Preferably, the ferric salt is at least one of ferrous sulfate heptahydrate, ferrous chloride, ferric sulfate, ferric chloride, ferric nitrate and ferric citrate; the nickel salt is at least one of nickel sulfate hexahydrate, nickel chloride, nickel nitrate and nickel acetate; the cobalt salt is at least one of cobalt chloride, cobalt sulfate, cobalt nitrate and cobalt acetate.
Preferably, in the step (1), the pH adjusting agent used for adjusting the pH value is at least one of sodium hydroxide, sodium bicarbonate, sodium carbonate and lime.
Preferably, in step (1), the stabilizer is at least one of lauryl acetic acid, gelatin, cysteine, diiodotyrosine, cystine and dimethyl dithio-carbamate; the complexing agent is at least one of polyvinylpyrrolidone, glycerol, ethylene diamine tetraacetic acid salt, sodium aminotriacetate, sodium pyrophosphate, ethylene diamine tetramethylene sodium phosphate, potassium pyrophosphate, diethylenetriamine pentacarboxylate and ammonium chloride; the surfactant is at least one of polystyrene, polyethylene glycol, sodium sulfamate, sodium dodecyl benzene sulfonate, 1, 4-butynediol, potassium sulfamate and palmitylamine bromide.
Preferably, in the step (2), the reducing agent is at least one of sodium borohydride, potassium borohydride, aluminum borohydride, hydrazine hydrate, hydrazine sulfate, formaldehyde or dimethyl ammonia borane.
Preferably, in the step (2), the solution is one of water, absolute ethyl alcohol or an aqueous solution of ethyl alcohol.
Preferably, in the step (3), the washing is performed by alternately washing with water and absolute ethyl alcohol until the pH value of the washing solution is neutral; the drying is specifically drying for 7-9 hours at 50-70 ℃ under the protection of nitrogen.
Preferably, in the step (2), the injection speed is 50-90 mL/s.
2. Ferromagnetic nanowires prepared by the method.
The invention has the beneficial effects that: the invention provides a preparation method of ferromagnetic nanowires and a product thereof, the method has simple synthetic route, controllable process, normal temperature and pressure reaction, meets the actual production requirement, is suitable for industrial production, and can overcome the defect that the traditional in-situ reduction method can only prepare ferromagnetic nanowires with a certain length-diameter ratio. When reducing agent solution with excessive concentration meets ferromagnetic metal salt, ferromagnetic ions can be reduced to generate ferromagnetic metal cores and generate a large number of bubbles. Meanwhile, the nanoscale ferromagnetic metal core can be self-assembled, namely, the ferromagnetic metal core is easy to be spontaneously or inductively assembled into the micro-nano particles with special shapes in the synthesis and growth processes. The reason for forming the shape of the nano-wire in the invention is that the injected reducing agent immediately reduces the surrounding ferromagnetic metal ions to generate ferromagnetic metal cores, and the ferromagnetic metal cores are converged and integrated into the nano-ball. Because the injected reducing agent is in columnar flow in the reaction solution, the ferromagnetic metal cores generated by reduction are also in columnar distribution, and adjacent spherical particles are mutually connected under the layer-by-layer deposition action of the ferromagnetic metal cores along with the growth of the nano spherical particles in the process of mutual aggregation and combination, so that the adjacent spherical particles are fused into a whole, and finally the nanowires with high length-diameter ratio are formed along the injected columnar flow. The ferromagnetic nanowire prepared by the method has good orientation, the diameter is less than 100nm, the length is 3-10 mu m, the length-diameter ratio is high, and the ferromagnetic nanowire has good flexibility, magnetic performance and microwave absorption performance.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
fig. 1 is an SEM image at 1.75 ten thousand times of ferromagnetic nanowires prepared in example 1;
fig. 2 is an SEM image at 10 ten thousand times of ferromagnetic nanowires prepared in example 1;
fig. 3 is an XRD pattern of the ferromagnetic nanowire prepared in example 1;
FIG. 4 is a graph of electromagnetic wave absorption curves of the ferromagnetic nanowires prepared in example 1;
fig. 5 is an SEM image at 2.79 ten thousand times of ferromagnetic nanowires prepared in example 1;
fig. 6 is an SEM image at 5 ten thousand times of ferromagnetic nanowires prepared in example 1;
fig. 7 is an SEM image of the ferromagnetic nanowires prepared in comparative example 1 under 12.4 ten thousand.
Detailed Description
The preferred embodiments of the present invention will be described in detail below.
Example 1
Preparation of ferromagnetic nanowires
1. A method of preparing ferromagnetic nanowires, the method comprising the steps of:
(1) dissolving ferromagnetic metal salt (ferrous sulfate heptahydrate) in deionized water, adjusting the pH value to 11 by using a pH regulator (sodium hydroxide), adding a stabilizer (gelatin), a complexing agent (polyvinylpyrrolidone) and a surfactant (polyethylene glycol), stirring, and introducing nitrogen to remove oxygen in the solution to form a ferrous sulfate heptahydrate mixed solution; the concentration of the ferrous sulfate heptahydrate in the ferrous sulfate heptahydrate mixed solution is 0.05mol/L, the concentration of gelatin is 0.02mol/L, the concentration of polyvinylpyrrolidone is 0.0015mol/L, and the concentration of polyethylene glycol is 0.0025 mol/L;
(2) dissolving a reducing agent (sodium borohydride) in deionized water to form a sodium borohydride solution; the concentration of sodium borohydride in the sodium borohydride solution is 1.2 mol/L;
(3) and (3) injecting the sodium borohydride solution formed in the step (2) into the ferrous sulfate heptahydrate mixed solution formed in the step (1) at the speed of 70mL/s by using an injector, reacting for 30min at 30 ℃ after the sodium borohydride solution is injected, collecting a solid product generated by the reaction by using a magnet, alternately cleaning the solid product by using water and absolute ethyl alcohol until the pH value of the cleaning solution is neutral, and drying for 8h at 60 ℃ under the protection of nitrogen, thus obtaining the sodium borohydride.
Example 2
1. A method of preparing ferromagnetic nanowires, the method comprising the steps of:
(1) dissolving ferromagnetic metal salt (ferric chloride) in deionized water, adjusting the pH value to 12 by using a pH regulator (sodium bicarbonate), adding a stabilizer (dodecyl acetic acid), a complexing agent (glycerol) and a surfactant (polystyrene), stirring, and introducing nitrogen to remove oxygen in the solution to form a ferric chloride mixed solution; the concentration of ferric chloride in the ferric chloride mixed solution is 0.08mol/L, the concentration of dodecyl acetic acid is 0.04mol/L, the concentration of glycerol is 0.001mol/L, and the concentration of polystyrene is 0.002 mol/L;
(2) dissolving a reducing agent (potassium borohydride) in absolute ethyl alcohol to form a potassium borohydride solution; the concentration of potassium borohydride in the potassium borohydride solution is 0.9 mol/L;
(3) and (3) injecting the potassium borohydride solution formed in the step (2) into the ferric chloride mixed solution formed in the step (1) at the speed of 50mL/s by using an injector, reacting for 45min at 20 ℃ after the injection of the potassium borohydride solution is finished, collecting a solid product generated by the reaction by using a magnet, alternately cleaning the solid product by using water and absolute ethyl alcohol until the pH value of a cleaning solution is neutral, and drying for 9h at 50 ℃ under the protection of nitrogen, thus obtaining the potassium borohydride.
Example 3
1. A method of preparing ferromagnetic nanowires, the method comprising the steps of:
(1) dissolving ferromagnetic metal salt (ferric citrate) in deionized water, adjusting the pH value to 10 by using a pH regulator (sodium carbonate), adding a stabilizer (dimethyl dithiocarbamate), a complexing agent (sodium aminotriacetate) and a surfactant (sodium dodecyl benzene sulfonate), stirring, and introducing nitrogen to remove oxygen in the solution to form a ferric citrate mixed solution; the concentration of ferric citrate in the ferric citrate mixed solution is 0.15mol/L, the concentration of dimethyl dithiocarbamate is 0.02mol/L, the concentration of sodium nitrilotriacetate is 0.002mol/L, and the concentration of sodium dodecyl benzene sulfonate is 0.003 mol/L;
(2) dissolving a reducing agent (hydrazine hydrate) in an ethanol aqueous solution formed by mixing absolute ethanol and deionized water according to the volume ratio of 1:1 to form a hydrazine hydrate solution; the concentration of hydrazine hydrate in the hydrazine hydrate solution is 2 mol/L;
(3) injecting the hydrazine hydrate solution formed in the step (2) into the ferric citrate mixed solution formed in the step (1) at a speed of 60mL/s by using an injector, after the injection of the hydrazine hydrate solution is finished, reacting for 40min at 40 ℃, collecting a solid product generated by the reaction by using a magnet, alternately cleaning the solid product by using water and absolute ethyl alcohol until the pH value of a cleaning solution is neutral, and drying for 7h at 60 ℃ under the protection of nitrogen, thus obtaining the hydrazine hydrate.
Example 4
1. A method of preparing ferromagnetic nanowires, the method comprising the steps of:
(1) dissolving ferromagnetic metal salt (ferric nitrate) in deionized water, adjusting the pH value to 12 by using a pH regulator (lime), adding a stabilizer (cystine), a complexing agent (sodium pyrophosphate) and a surfactant (1, 4-butynediol), stirring, and introducing nitrogen to remove oxygen in the solution to form a ferric nitrate mixed solution; the concentration of ferric nitrate in the ferric nitrate mixed solution is 0.1mol/L, the concentration of cystine is 0.03mol/L, the concentration of sodium pyrophosphate is 0.001mol/L, and the concentration of 1,4 butynediol is 0.002 mol/L;
(2) dissolving a reducing agent (aluminum borohydride) in absolute ethyl alcohol to form an aluminum borohydride solution; the concentration of aluminum borohydride in the aluminum borohydride solution is 1.5 mol/L;
(3) and (3) injecting the aluminum borohydride solution formed in the step (2) into the ferric nitrate mixed solution formed in the step (1) at a speed of 90mL/s by using an injector, reacting for 35min at 30 ℃ after the injection of the aluminum borohydride solution is finished, collecting a solid product generated by the reaction by using a magnet, alternately cleaning the solid product by using water and absolute ethyl alcohol until the pH value of a cleaning solution is neutral, and drying for 8h at 65 ℃ under the protection of nitrogen, thus obtaining the aluminum borohydride.
Example 5
1. A method of preparing ferromagnetic nanowires, the method comprising the steps of:
(1) dissolving ferromagnetic metal salt (ferric sulfate) in deionized water, adjusting the pH value to 10 by using a pH regulator (sodium hydroxide), adding a stabilizer (diiodotyrosine), a complexing agent (ammonium chloride) and a surfactant (sodium sulfamate), stirring, and introducing nitrogen to remove oxygen in the solution to form a ferric sulfate mixed solution; the ferric sulfate concentration of the ferric sulfate mixed solution is 0.09mol/L, the diiodotyrosine concentration is 0.04mol/L, the ammonium chloride concentration is 0.001mol/L, and the sodium sulfamate concentration is 0.003 mol/L;
(2) dissolving a reducing agent (hydrazine sulfate) in deionized water to form a hydrazine sulfate solution; the concentration of hydrazine sulfate in the hydrazine sulfate solution is 1.8 mol/L;
(3) injecting the hydrazine sulfate solution formed in the step (2) into the ferric sulfate mixed solution formed in the step (1) at a speed of 80mL/s by using an injector, after the injection of the hydrazine sulfate solution is finished, reacting for 30min at 35 ℃, collecting a solid product generated by the reaction by using a magnet, alternately cleaning the solid product by using water and absolute ethyl alcohol until the pH value of a cleaning solution is neutral, and drying for 8h at 60 ℃ under the protection of nitrogen, thus obtaining the hydrazine sulfate.
Comparative example 1
The difference from example 1 is that the sodium borohydride solution formed in step (2) is dropped into the ferrous sulfate heptahydrate mixed solution formed in step (1) in a dropping manner.
The ferromagnetic nanowires prepared in example 1 are detected by a scanning electron microscope under the magnification of 1.75 ten thousand times and 10 ten thousand times respectively, and the test results are shown in fig. 1 and fig. 2, wherein fig. 1 is an SEM image under 1.75 ten thousand times, and fig. 2 is an SEM image under 10 ten thousand times, and as can be seen from fig. 1 and fig. 2, the ferromagnetic nanowires prepared in example 1 have better dispersibility, the diameter is less than 100nm, and the length is 3-10 μm.
The X-ray diffraction was performed on the ferromagnetic nanowire prepared in example 1, and the test result is shown in fig. 3, as can be seen from fig. 3, the spectrum of the diffraction peak of the ferromagnetic nanowire is identical to the peak value of the standard diffraction spectrum (JCPDS card No.06-0696), which indicates that the prepared product is composed of elemental iron and no impurity peak appears, and indicates that the purity of the ferromagnetic nanowire in the tested sample is high and close to 100%.
The sample containing 40 wt% of the ferromagnetic nanowire in the embodiment 1 is prepared, and the test result is shown in fig. 4 by testing in a range of 2-18 GHz by a coaxial method, as can be seen from fig. 4, the minimum reflection loss reaches-18 dB, the effective absorption range with the reflection loss smaller than-10 dB is 7.02-9.58 GHz, and the range amplitude reaches 2.56GHz, which indicates that the ferromagnetic nanowire prepared by the method has excellent electromagnetic shielding and wave absorbing properties.
The ferromagnetic nanowires prepared in example 3 are detected by a scanning electron microscope under the magnifications of 2.79 ten thousand times and 5 ten thousand times respectively, and the test results are shown in fig. 5 and fig. 6, wherein fig. 5 is an SEM image under 2.79 ten thousand times, and fig. 6 is an SEM image under 5 ten thousand times, and it can be seen from fig. 5 and fig. 6 that the ferromagnetic nanowires prepared in example 3 have better dispersibility, the diameter is less than 100nm, and the length is 3-10 μm.
The ferromagnetic nanowires prepared in comparative example 1 were examined by scanning electron microscopy at a magnification of 12.4 ten thousand times, and the results are shown in fig. 7, and it can be seen from fig. 7 that the ferromagnetic nanowires prepared in comparative example 1 have a smaller aspect ratio and are more curved.
In the present invention, in addition to the iron salt, one of nickel salt and cobalt salt may be used, and the same technical effects can be achieved.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (9)
1. A method for preparing ferromagnetic nanowires, characterized in that the method comprises the following steps:
(1) dissolving ferromagnetic metal salt in water, then adjusting the pH value to 10-12, adding a stabilizer, a complexing agent and a surfactant, stirring, and removing oxygen in the solution to form a ferromagnetic metal salt mixed solution; the concentration of the ferromagnetic metal salt in the ferromagnetic metal salt mixed solution is 0.05-0.15 mol/L, the concentration of the stabilizer is 0.02-0.04 mol/L, the concentration of the complexing agent is 0.001-0.002 mol/L, and the concentration of the surfactant is 0.002-0.003 mol/L;
(2) dissolving a reducing agent in the solution to form a reducing agent solution; the concentration of the reducing agent in the reducing agent solution is 0.9-2 mol/L;
(3) injecting the reducing agent solution formed in the step (2) into the ferromagnetic metal salt mixed solution formed in the step (1), reacting for 30-45 min at 20-40 ℃ after the injection of the reducing agent solution is finished, obtaining a solid product, and cleaning and drying the solid product; the injection speed is 50-90 mL/s.
2. The method according to claim 1, wherein in step (1), the ferromagnetic metal salt is one of iron salt, nickel salt or cobalt salt.
3. The method of claim 2, wherein the iron salt is at least one of ferrous sulfate heptahydrate, ferrous chloride, ferric sulfate, ferric chloride, ferric nitrate, and ferric citrate; the nickel salt is at least one of nickel sulfate hexahydrate, nickel chloride, nickel nitrate and nickel acetate; the cobalt salt is at least one of cobalt chloride, cobalt sulfate, cobalt nitrate and cobalt acetate.
4. The method according to claim 1, wherein in the step (1), the pH adjusting agent used for adjusting the pH value is at least one of sodium hydroxide, sodium bicarbonate, sodium carbonate and lime.
5. The method according to claim 1, wherein in step (1), the stabilizer is at least one of lauryl acetic acid, gelatin, cysteine, diiodotyrosine, cystine, dimethyl dithio-carbamate; the complexing agent is at least one of polyvinylpyrrolidone, glycerol, ethylene diamine tetraacetic acid salt, sodium aminotriacetate, sodium pyrophosphate, ethylene diamine tetramethylene sodium phosphate, potassium pyrophosphate, diethylenetriamine pentacarboxylate and ammonium chloride; the surfactant is at least one of polystyrene, polyethylene glycol, sodium sulfamate, sodium dodecyl benzene sulfonate, 1, 4-butynediol, potassium sulfamate and palmitylamine bromide.
6. The method according to claim 1, wherein in the step (2), the reducing agent is at least one of sodium borohydride, potassium borohydride, aluminum borohydride, hydrazine hydrate, hydrazine sulfate, formaldehyde or dimethyl ammonia borane.
7. The method of claim 1, wherein in step (2), the solution is one of water, absolute ethanol, or an aqueous solution of ethanol.
8. The method according to claim 1, wherein in the step (3), the washing is carried out by alternately washing with water and absolute ethyl alcohol until the pH value of the washing liquid is neutral; the drying is specifically drying for 7-9 hours at 50-70 ℃ under the protection of nitrogen.
9. Ferromagnetic nanowires produced by the method of any one of claims 1 to 8.
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