CN101880917A - Method for preparing nano ceramic fibers - Google Patents
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Abstract
The invention discloses a method for preparing nano ceramic fibers, which is implemented by the following steps: 1, preparing 3 to 15 volume percent of 10 to 30 nanometer ceramic nanoparticles, 5 to 30 volume percent of spinnable high polymer, 0.5 to 5 volume percent of dispersant and the balance of solvent, wherein the total volume of the raw materials is 100 volume percent; 2, adding the spinnable high polymer into the solvent, heating the mixture in a water bath with magnetic stirring to obtain solution of spinnable high polymer; 3, adding the ceramic nanoparticles and the dispersant into the solution of spinnable high polymer obtained by the step 2, keeping the temperature of the mixture constant in a water bath, performing dispersion and ultrasonic dispersion, and performing swelling at a constant temperature to obtain ceramic nanoparticle/spinnable high polymer/solvent spinning solution; 4, controlling the electrostatic spinning process parameters of the spinning solution obtained by the step 3 to obtain nano fibers; and 5, sintering the nano fibers at 400 to 1,200 DEG C to obtain nano ceramic fibers.
Description
Technical field
The invention belongs to nano ceramic material manufacturing technology field, relate to a kind of method for preparing nano ceramic fibers.
Background technology
Nano ceramic fibers is the material that a class serves many purposes, and is widely used in fields such as catalysis, purification, atmosphere storage, sensor and environmental protection.Mainly utilize the loose structure of nano ceramic fibers and huge specific area, the character of bond material itself obtains needed various physics and chemical property.The purposes difference of nano ceramic fibers has proposed different requirements to its diameter, structure etc.
The preparation method of nano ceramic fibers has a lot, as hydrothermal synthesis method, chemical vapour deposition technique, chemical gas-phase reaction method, organic polymer precursor body conversion method, template etc., all can prepare the nano ceramic fibers that diameter is tiny, draw ratio is high.But there are shortcomings such as diameter skewness, pliability is poor, the preparation route is long in the fiber that these methods are produced, and the appearance of electrostatic spinning technique has remedied above deficiency.The electrostatic spinning processing method has equipment simple, with low cost, operation and advantage such as efficient easily, has caused the extensive concern of various countries' researchers.The core of electrostatic spinning technique is to make charged Polymer Solution or melt flow deformation in electrostatic field, and evaporation of process solvent or melt cool off and solidify then, obtain fibrous material.
At present, the main method that electrostatic spinning prepares nano ceramic fibers is can spin high polymer to be dissolved in solvent, obtain to spin high polymeric solution, add ceramic forerunner then, obtain spinning solution after the stirring, obtain ceramic forerunner/can spin the high polymer nano fiber by electrostatic spinning technique then, obtain nano ceramic fibers behind the high temperature sintering.But the precondition of this method is that pottery must have presoma also can mix with high polymer, makes spinnable solution, has limited the kind of electrospinning nano ceramic fibers, and the nano ceramic fibers that can prepare is of less types, can not satisfy the demand of practical application.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing nano ceramic fibers, solved the raw material configuration condition strictness of the electrospinning nano ceramic fibers that exists in the prior art, the kind of selecting materials restriction is big, and the nano ceramic fibers that can prepare is of less types, problem that can not practical requirement.
The technical solution adopted in the present invention is, a kind of method for preparing nano ceramic fibers, and this method is implemented according to following steps:
Step 1: percentage by volume, getting particle diameter is the ceramic nano particle 3%-15% of 10nm-300nm, can spin high polymer 5%-30%, dispersant 0.5%-5%, all the other are solvent, cumulative volume is 100%;
Step 2: the spun high polymer of obtaining in the step 1 is joined in the solvent, and heating and magnetic agitation make viscosity and can spin high polymeric solution uniformly in water-bath;
Step 3: join ceramic nano particle and the dispersant obtained in the step 1 in the spun high polymeric solution that obtains in the step 2 simultaneously, in water-bath, keep constant temperature, then solution is disperseed, need to continue to stir 0.5-1h, then mixed solution is carried out ultrasonic dispersing 0.5-1h, and at 50-75 ℃ of constant temperature swelling 0.5-1h, the uniform ceramic nano particle of formation composition/can spin high polymer/solvent spinning solution;
Step 4: pour the spinning solution that obtains in the step 3 into syringe, the injection needle that employing is scabbled is as the capillary that sprays thread, voltage is 10-40kV in the electrostatic spinning process, collecting distance is 10-30cm, the spinning solution fltting speed is 0.5-2.5mL/h, environment temperature is 10-50 ℃, and ambient humidity is 50%-75%, is prepared into ceramic nano particle/can spin the high polymer nano fiber through electrostatic spinning technique;
Step 5: the nanofiber that obtains in the step 4 through 400 ℃ of-1200 ℃ of sintering, is obtained nano ceramic fibers.
The nano ceramic fibers that the invention has the beneficial effects as follows preparation is of a great variety, can prepare the nanofiber of most of ceramic materials, the distribution of fiber diameters that obtains is average, the draw ratio height, pliability is good, preparation technology is simple, and product success rate height can be widely used in fields such as filtering material, sensor material, fibre reinforcement, catalyst, drug release carrier, fuel cell, solar energy sensitization battery, artificial bone alternative materials.
The specific embodiment
The present invention is described in detail below in conjunction with the specific embodiment.
The preparation method of nano ceramic fibers of the present invention, implement according to following steps:
Step 1: percentage by volume, getting particle diameter is the ceramic nano particle 3%-15% of 10nm-300nm, can spin high polymer 5%-30%, dispersant 0.5%-5%, all the other are solvent, cumulative volume is 100%.
The ceramic nano particle is chosen: a kind of in titanium dioxide, zinc oxide, magnesia, calcium oxide, zirconium dioxide, vanadic anhydride, iron oxide, cobalt oxide, nickel oxide, aluminium oxide, manganese dioxide, boron oxide, tin ash, lead oxide, arsenic oxide arsenoxide, chromium oxide, cadmium oxide, carborundum, silicon nitride, boron nitride, inorganic carbide, the inorganic nitride.
Can spin high polymer chooses: a kind of in polyvinylpyrrolidone, polyethylene glycol, polyvinyl butyral resin, Sodium Polyacrylate, polymethyl methacrylate, polyvinyl alcohol, cellulose, Merlon, metaphenylene isophthaloyl amine, elasticity polypeptide, recombinant protein, polyimides, PLA, the polybenzimidazoles.
Dispersant is chosen: a kind of in aliphatic acid, softex kw, silicate, sodium aluminate, ammonium citrate, aluminic acid ester, polyethylene glycol (4000), ten diaminourea sodium sulphate, vinyl acetate, propionate, ammonium polymethacrylate, adipic acid, stearic acid, polymine, ammonium acrylate, acrylic acid, methyl esters, resin acid, polyethers, calgon, sodium chloride, potassium nitrate, natrium citricum, hydrated silica, the water-soluble organic silicon.
Solvent is chosen: water, ethanol, acetone, chloroform, isopropyl alcohol, methyl alcohol, toluene, oxolane, benzene, benzylalcohol 1,4-diox, propyl alcohol, carrene, carbon tetrachloride, cyclohexane, ring ethyl ketone, phenol, pyridine, trichloroethanes, acetate, hexafluoroisopropanol, Hexafluoro acetone, acetonitrile, N-methylmorpholine-N-oxide, 1, a kind of in 3-dioxolanes, methyl ethyl ketone, the N-Methyl pyrrolidone.
Step 2: the spun high polymer of obtaining in the step 1 is joined in the solvent, and heating and magnetic agitation make viscosity and can spin high polymeric solution uniformly in water-bath.
Step 3: join ceramic nano particle and the dispersant obtained in the step 1 in the spun high polymeric solution that obtains in the step 2 simultaneously, in the water-bath of uniform temperature, keep constant temperature, then solution is disperseed, for preventing hot-spot and accelerating the ceramic nano Dispersion of Particles, need to continue to stir 0.5-1h, then mixed solution is carried out ultrasonic dispersing 0.5-1h, and at 50-75 ℃ of constant temperature swelling 0.5-1h, the uniform ceramic nano particle of formation composition/can spin high polymer/solvent spinning solution.
Step 4: pour the spinning solution that obtains in the step 3 into syringe, the injection needle that employing is scabbled is as the capillary that sprays thread, voltage is 10-40kV in the electrostatic spinning process, collecting distance is 10-30cm, the spinning solution fltting speed is 0.5-2.5mL/h, environment temperature is 10-50 ℃, and ambient humidity is 50%-75%, is prepared into ceramic nano particle/can spin the high polymer nano fiber through electrostatic spinning technique.
Step 5: the 400-1200 ℃ of sintering of nanofiber process with obtaining in the step 4 obtains nano ceramic fibers.
The principle that the present invention prepares nano ceramic fibers is:
At first, can the ceramic nano particle play a decisive role to finally obtaining nano ceramic fibers with the ratio that can spin high polymer.If the ceramic nano proportion of particles is little, then can't obtain continuous ceramic nanofibers; If ratio is big, then in the electrostatic spinning process, can't prepare nanofiber.
Secondly, the present invention is than existing electrospinning nano ceramic fibers technology of preparing, in the preparation process of spinning solution the ceramic nano particle being joined to spin in the high polymeric solution, do not need ceramic forerunner, the nano ceramic fibers that obtains can be the ceramic material of no presoma and the ceramic material that presoma can not be made spinnable solution with high polymer, has increased the preparation kind of electrospinning nano ceramic fibers.
Once more, the adding of dispersant can make between the ceramic nano particle and have repulsive force, change the particle surface functional group, strengthen the wettability of solid to solvent, solve nanoparticle agglomerates, disperseed unequal problem, the spinning solution ceramic nano particle in spinning process that obtains can not precipitated, can keep the composition of spinning solution even.By ultrasonic wave the mixed solution that contains the ceramic nano particle is disperseed, be distributed in the mixed solution with can making the ceramic nano uniform particles, obtain the uniform spinning solution of composition.The constant temperature swelling process can and can spin high polymer with ceramic nanofibers and better combine, and helps follow-up preparation.
At last, adopt electrostatic spinning technique to obtain ceramic nano particle/can spin the high polymer nano fiber, and obtain nano ceramic fibers through oversintering.
Embodiment 1
By volume percentage is got the Si that particle diameter is 10nm
3N
4Nano particle 3%, polyvinyl alcohol (PVA) is 10%, softex kw 0.5% and 86.5% deionized water, cumulative volume is 100%.(PVA) joins in the deionized water with polyvinyl alcohol, and heating and magnetic agitation make the PVA solution with certain viscosity in 85 ℃ of water-baths; With Si
3N
4Nano particle and softex kw join in the PVA solution, keep 85 ℃ of constant temperature in water-bath, then solution are disperseed, continue to stir 1h, then mixed solution is carried out ultrasonic dispersing 0.5h, and, form the uniform Si of composition at 50 ℃ of constant temperature swelling 0.5h
3N
4/ PVA spinning solution.Pour spinning solution into syringe, adopt the injection needle that scabbles as the capillary that sprays thread, voltage is 10kV in the electrostatic spinning process, collecting distance is 10cm, and the spinning solution fltting speed is 0.5mL/h, and environment temperature is 10 ℃, ambient humidity is 50%, is prepared into Si through electrostatic spinning technique
3N
4/ PVA composite nano fiber; Through 400 ℃ of sintering, obtain nanometer Si at last
3N
4Fiber.
Under same composition and the experiment condition, the nanofiber important technological parameters that the inventive method and existing method obtain sees Table 1 embodiment 1.
Embodiment 2
Percentage by volume, getting particle diameter is the NiO nano particle 6% of 300nm, polyvinyl butyral resin (PVB) is 5%, ammonium citrate 5% and 84% deionized water, cumulative volume is 100%.(PVB) joins in the ethanol with polyvinyl butyral resin, and heating and magnetic agitation make the PVB solution with certain viscosity in 75 ℃ of water-baths; NiO nano particle and ammonium citrate are joined in the PVB solution, in water-bath, keep 50 ℃ of constant temperature, then solution is disperseed, continue to stir 1h, then mixed solution is carried out ultrasonic dispersing 0.5h, and, form the uniform NiO/PVB spinning solution of composition at 75 ℃ of constant temperature swelling 0.5h.Pour spinning solution into syringe, the injection needle that employing is scabbled is as the capillary that sprays thread, voltage is 40kV in the electrostatic spinning process, collecting distance is 30cm, the spinning solution fltting speed is 2.5mL/h, environment temperature is 50 ℃, and ambient humidity is 75%, is prepared into the NiO/PVB composite nano fiber through electrostatic spinning technique; Through 500 ℃ of sintering, obtain the nano NiO fiber at last.
Under same composition and the experiment condition, the nanofiber important technological parameters that the inventive method and existing method obtain sees Table 1 embodiment 2.
Embodiment 3
By volume percentage is got the B that particle diameter is 200nm
4N nano particle 15%, polyvinylpyrrolidone (PVP) is 20%, polyethers 3% and 62% ethanol, cumulative volume is 100%.(PVP) joins in the isopropyl alcohol with polyvinylpyrrolidone, and heating and magnetic agitation make the PVP solution with certain viscosity in 70 ℃ of water-baths; With B
4N nano particle and polyethers join in the PVP solution, keep 60 ℃ of constant temperature in water-bath, then solution are disperseed, for preventing hot-spot and accelerating B
4The N nanoparticulate dispersed needs to continue to stir 0.5h, then mixed solution is carried out ultrasonic dispersing 1h, and at 60 ℃ of constant temperature swelling 1h, forms the uniform B of composition
4The N/PVP spinning solution.Pour spinning solution into syringe, adopt the injection needle that scabbles as the capillary that sprays thread, voltage is 30kV in the electrostatic spinning process, collecting distance is 20cm, and the spinning solution fltting speed is 2mL/h, and environment temperature is 40 ℃, ambient humidity is 65%, is prepared into B through electrostatic spinning technique
4The N/PVP composite nano fiber; Through 600 ℃ of sintering, obtain nanometer B at last
4The N fiber.
Under same composition and the experiment condition, the nanofiber important technological parameters that the inventive method and existing method obtain sees Table 1 embodiment 3.
Embodiment 4
Percentage by volume, getting particle diameter is the CuO nano particle 8% of 150nm, polymethyl methacrylate (PMMA) is 10%, propionate 2% and 80% isopropyl alcohol, cumulative volume is 100%.(PMMA) joins in the isopropyl alcohol with polymethyl methacrylate, and heating and magnetic agitation make the PMMA solution with certain viscosity in water-bath; CuO nano particle and propionate are joined in the PMMA solution, in water-bath, keep 90 ℃ of constant temperature, then solution is disperseed, continue to stir 1h, then mixed solution is carried out ultrasonic dispersing 1h, and, form the uniform CuO/PMMA spinning solution of composition at 50 ℃ of constant temperature swelling 1h.Pour spinning solution into syringe, the injection needle that employing is scabbled is as the capillary that sprays thread, voltage is 25kV in the electrostatic spinning process, collecting distance is 25cm, the spinning solution fltting speed is 1.5mL/h, environment temperature is 25 ℃, and ambient humidity is 55%, is prepared into the CuO/PMMA composite nano fiber through electrostatic spinning technique; Through 800 ℃ of sintering, obtain nanometer CuO fiber.
Under same composition and the experiment condition, the nanofiber important technological parameters that the inventive method and existing method obtain sees Table 1 embodiment 4.
Embodiment 5
By volume percentage is got the SnO that particle diameter is 250nm
2Nano particle 5%, Sodium Polyacrylate (PAAS) is 15%, ammonium polymethacrylate 1% and 79% deionized water, cumulative volume is 100%.(PAAS) joins in the deionized water with Sodium Polyacrylate, and heating and magnetic agitation make the PAAS solution with certain viscosity in water-bath.With SnO
2Nano particle and ammonium polymethacrylate join in the PAAS solution, keep 90 ℃ of constant temperature in water-bath, then solution are disperseed, continue to stir 0.5h, then mixed solution is carried out ultrasonic dispersing 0.5h, and, form the uniform SnO of composition at 75 ℃ of constant temperature swelling 0.5h
2/ PAAS spinning solution.Pour spinning solution into syringe, adopt the injection needle that scabbles as the capillary that sprays thread, voltage is 15kV in the electrostatic spinning process, collecting distance is 15cm, and the spinning solution fltting speed is 1mL/h, and environment temperature is 15 ℃, ambient humidity is 70%, is prepared into SnO through electrostatic spinning technique
2/ PAAS composite nano fiber; Through 1000 ℃ of sintering, obtain nano SnO
2Fiber.
Under same composition and the experiment condition, the nanofiber important technological parameters that the inventive method and existing method obtain sees Table 1 embodiment 5.
Embodiment 6
Percentage by volume, getting particle diameter is the SiC nano particle 10% of 180nm, polyethylene glycol (PEG) is 30%, polymine 4% and 56% pyridine, cumulative volume is 100%.(PEG) joins in the pyridine with polyethylene glycol, and heating and magnetic agitation make the PEG solution with certain viscosity in 85 ℃ of water-baths; SiC nano particle and polymine are joined in the PEG solution, in water-bath, keep 85 ℃ of constant temperature, then solution is disperseed, continue to stir 0.5h, then mixed solution is carried out ultrasonic dispersing 1h, and, form the uniform SiC/PEG spinning solution of composition at 60 ℃ of constant temperature swelling 1h.Pour spinning solution into syringe, the injection needle that employing is scabbled is as the capillary that sprays thread, voltage is 35kV in the electrostatic spinning process, collecting distance is 25cm, the spinning solution fltting speed is 0.8mL/h, environment temperature is 45 ℃, and ambient humidity is 72%, is prepared into the SiC/PEG composite nano fiber through electrostatic spinning technique; Through 1100 ℃ of sintering, obtain the nano SiC fiber at last.
Under same composition and the experiment condition, the nanofiber important technological parameters that the inventive method and existing method obtain sees Table 1 embodiment 6.
Embodiment 7
By volume percentage is got the Al that particle diameter is 100nm
2O
3Nano particle 15%, Merlon (PC) is 10%, and aluminic acid ester 2.5% and toluene are 72.5%, and cumulative volume is 100%.(PC) joins in the toluene with Merlon, and heating and magnetic agitation make the PC solution with certain viscosity in water-bath; With Al
2O
3Nano particle and aluminic acid ester join in the PC solution, keep 85 ℃ of constant temperature in water-bath, then solution are disperseed, and continue to stir 1h, then mixed solution are carried out ultrasonic dispersing 0.5h, and at 65 ℃ of constant temperature swelling 0.5h, form the uniform Al of composition
2O
3/ PC spinning solution.Pour spinning solution into syringe, adopt the injection needle that scabbles as the capillary that sprays thread, voltage is 40kV in the electrostatic spinning process, collecting distance is 10cm, and the spinning solution fltting speed is 2.5mL/h, and environment temperature is 10 ℃, ambient humidity is 50%, is prepared into Al through electrostatic spinning technique
2O
3/ PC composite nano fiber; At last with composite nano fiber through 1200 ℃ of sintering, obtain nanometer Al
2O
3Fiber.
Under same composition and the experiment condition, the nanofiber important technological parameters that the inventive method and existing method obtain sees Table 1 embodiment 7.
Embodiment 8
By volume percentage is got the TiO that particle diameter is 50nm
2Nano particle 8%, polyvinylpyrrolidone (PVP) 10%, calgon 2%, ethanol 80%, cumulative volume are 100%.(PVP) joins in the solvent with polyvinylpyrrolidone, keeps 60 ℃ of constant temperature in water-bath, continues to stir 0.5h, makes the PVP/ ethanolic solution; With TiO
2Nano particle and calgon join in the PVP/ ethanolic solution, keep 50 ℃ of constant temperature in water-bath, then solution are disperseed, for preventing hot-spot and accelerating TiO
2Nanoparticulate dispersed needs to continue to stir 1h, then mixed solution is carried out ultrasonic dispersing 1h, and 55 ℃ of constant temperature swelling 0.5h, forms the uniform TiO of composition
2/ PVP/ ethanol spinning solution; With TiO
2/ PVP/ ethanol spinning solution is poured syringe into, the injection needle that employing is scabbled is as the capillary that sprays thread, voltage is 40kV in the electrostatic spinning process, collecting distance is 10cm, the spinning solution fltting speed is 2.5mL/h, environment temperature is 10 ℃, and ambient humidity is 75%, is prepared into TiO through electrostatic spinning technique
2/ PV nanofiber through 1000 ℃ of sintering, finally obtains TiO
2Nanofiber.
Under same composition and the experiment condition, the nanofiber important technological parameters that the inventive method and existing method obtain sees Table 1 embodiment 8.
Each embodiment the present invention of table 1 prepares and has the nanofiber feature comparison sheet that method obtains now
The nano ceramic fibers kind that the inventive method can prepare significantly increases, can prepare the nanofiber of most of ceramic materials, the distribution of fiber diameters that obtains is average, the draw ratio height, pliability is good, related Experiment Preparation technology is simple, and product success rate height can be widely used in fields such as filtering material, sensor material, fibre reinforcement, catalyst, drug release carrier, fuel cell, solar energy sensitization battery, artificial bone alternative materials.
Claims (5)
1. a method for preparing nano ceramic fibers is characterized in that, this method is implemented according to following steps:
Step 1: percentage by volume, getting particle diameter is the ceramic nano particle 3%-15% of 10nm-300nm, can spin high polymer 5%-30%, dispersant 0.5%-5%, all the other are solvent, cumulative volume is 100%;
Step 2: the spun high polymer of obtaining in the step 1 is joined in the solvent, and heating and magnetic agitation make viscosity and can spin high polymeric solution uniformly in water-bath;
Step 3: join ceramic nano particle and the dispersant obtained in the step 1 in the spun high polymeric solution that obtains in the step 2 simultaneously, in water-bath, keep constant temperature, then solution is disperseed, need to continue to stir 0.5-1h, then mixed solution is carried out ultrasonic dispersing 0.5-1h, and at 50-75 ℃ of constant temperature swelling 0.5-1h, the uniform ceramic nano particle of formation composition/can spin high polymer/solvent spinning solution;
Step 4: pour the spinning solution that obtains in the step 3 into syringe, the injection needle that employing is scabbled is as the capillary that sprays thread, voltage is 10-40kV in the electrostatic spinning process, collecting distance is 10-30cm, the spinning solution fltting speed is 0.5-2.5mL/h, environment temperature is 10-50 ℃, and ambient humidity is 50%-75%, is prepared into ceramic nano particle/can spin the high polymer nano fiber through electrostatic spinning technique;
Step 5: the nanofiber that obtains in the step 4 through 400 ℃ of-1200 ℃ of sintering, is obtained nano ceramic fibers.
2. method according to claim 1, it is characterized in that described ceramic nano particle is chosen: a kind of in titanium dioxide, zinc oxide, magnesia, calcium oxide, zirconium dioxide, vanadic anhydride, iron oxide, cobalt oxide, nickel oxide, aluminium oxide, manganese dioxide, boron oxide, tin ash, lead oxide, arsenic oxide arsenoxide, chromium oxide, cadmium oxide, carborundum, silicon nitride, boron nitride, inorganic carbide or the inorganic nitride.
3. method according to claim 1, it is characterized in that the described high polymer that spins is chosen: a kind of in polyvinylpyrrolidone, polyethylene glycol, polyvinyl butyral resin, Sodium Polyacrylate, polymethyl methacrylate, polyvinyl alcohol, cellulose, Merlon, metaphenylene isophthaloyl amine, elasticity polypeptide, recombinant protein, polyimides, PLA or the polybenzimidazoles.
4. method according to claim 1, it is characterized in that described dispersant is chosen: a kind of in aliphatic acid, softex kw, silicate, sodium aluminate, ammonium citrate, aluminic acid ester, polyethylene glycol, ten diaminourea sodium sulphate, vinyl acetate, propionate, ammonium polymethacrylate, adipic acid, stearic acid, polymine, ammonium acrylate, acrylic acid, methyl esters, resin acid, polyethers, calgon, sodium chloride, potassium nitrate, natrium citricum, hydrated silica or the water-soluble organic silicon.
5. method according to claim 1, it is characterized in that, described solvent is chosen: water, ethanol, acetone, chloroform, isopropyl alcohol, methyl alcohol, toluene, oxolane, benzene, benzylalcohol 1,4-diox, propyl alcohol, carrene, carbon tetrachloride, cyclohexane, ring ethyl ketone, phenol, pyridine, trichloroethanes, acetate, hexafluoroisopropanol, Hexafluoro acetone, acetonitrile, N-methylmorpholine N oxide, 1, a kind of in 3-dioxolanes, methyl ethyl ketone or the N methyl pyrrolidone.
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