The preparation method of six side's mangaic acid yttrium nanofibers
Technical field
The present invention relates to a kind of preparation method of nanofiber, particularly a kind of preparation method of six side's mangaic acid yttrium nanofibers.
Background technology
Multi-ferroic material is widely used in numerous areas such as storage storage and transmitter, is a kind of very important functional material.Six side's mangaic acid yttrium materials are not because it contains any volatile element, and have only advantage such as single polaxis, and development is very fast in the past ten years.
Document " K.Kim; C.Kim; The effects of drying temperature on the crystallization of YMnO3 thin films prepared by sol-gel method using alkoxides; J.Eur.Ceram.Soc.2004; 24:2613-2617 " discloses a kind of method that adopts Prepared by Sol Gel Method mangaic acid yttrium material, at first go out colloid with preparation of raw material, evenly be spin-coated in the substrate then, in retort furnace, be incubated at last, can obtain mangaic acid yttrium material.But this method can only be prepared the mangaic acid yttrium material of micron number magnitude, can't prepare the mangaic acid yttrium material of the nanometer scale that adapts to modern development in science and technology.
Summary of the invention
In order to overcome the big deficiency of mangaic acid yttrium material particle size that prior preparation method is prepared, the invention provides a kind of preparation method of six side's mangaic acid yttrium nanofibers.This method is dissolved into citric acid and forms citric acid solution in the deionized water; Again with Y (NO
3)
3, Mn (CH
3COO)
2Add to stir to clarify in the citric acid solution transparent, solution left standstill is placed on heated and stirred in the water-bath after placing, in solution, add polyvinylpyrrolidone, continuing to be stirred to polyvinylpyrrolidone dissolves fully, the concentration that keeps polyvinylpyrrolidone, utilize syringe pump and high-voltage power supply to carry out electrostatic spinning, collect fiber with monocrystalline silicon piece; The fiber of collecting placed put into retort furnace insulation calcining after the loft drier drying, obtain six side's mangaic acid yttrium nanofibers.
The technical solution adopted for the present invention to solve the technical problems: a kind of preparation method of six side's mangaic acid yttrium nanofibers is characterized in comprising the steps:
(a) with C
6H
8O
7Being dissolved into and forming concentration in the deionized water is the C of 0.2~0.4g/mL
6H
8O
7Solution;
(b) with Y (NO
3)
3, Mn (CH
3COO)
2Add to stir to clarify in the citric acid solution transparent, Y (NO wherein
3)
36H
2O: Mn (CH
3COO)
24H
2O: C
6H
8O
7Mol ratio=1: 1: 2;
(c) place through the solution left standstill of step (b) preparation and be placed on after 24~72 hours in the water-bath in 50~90 ℃ of heated and stirred 3~7 hours, add molecular weight then and be 1.3 * 106 polyvinylpyrrolidone, continue to be stirred to polyvinylpyrrolidone and dissolve fully, make the concentration of polyvinylpyrrolidone remain on 0.02~0.05g/mL;
(d) adding the high polymeric solution of step (c) preparation to internal diameter is 1~3mm, syringe needle is in the plastic injector of stainless steel syringe needle, syringe is added in the syringe pump, it is 0.3~0.7mL/h that the startup syringe pump makes the injection flow velocity, open high-voltage power supply simultaneously and provide the voltage of 20~30kV, collect fiber with monocrystalline silicon piece to syringe needle;
(e) fiber of collecting is placed loft drier put into retort furnace after 4~8 hours, be warming up to 1000~1400 ℃ with the heat-up rate of 1~5 ℃/min 100~150 ℃ of dryings, and insulation calcining 6~12 hours, six side's mangaic acid yttrium nanofibers obtained.
The invention has the beneficial effects as follows: because this method is dissolved into citric acid and forms citric acid solution in the deionized water; Again with Y (NO
3)
3, Mn (CH
3COO)
2Add to stir to clarify in the citric acid solution transparent, solution left standstill is placed on heated and stirred in the water-bath after placing, in solution, add polyvinylpyrrolidone, continuing to be stirred to polyvinylpyrrolidone dissolves fully, the concentration that keeps polyvinylpyrrolidone, utilize syringe pump and high-voltage power supply to carry out electrostatic spinning, collect fiber with monocrystalline silicon piece; The fiber of collecting placed put into retort furnace insulation calcining after the loft drier drying, obtain six side's mangaic acid yttrium nanofibers.
Below in conjunction with the drawings and specific embodiments the present invention is elaborated.
Description of drawings
The XRD figure spectrum of the prepared six side's mangaic acid yttrium nanofibers of Fig. 1 the inventive method.
The degradation rate of the tropeolin-D that the prepared six side's mangaic acid yttrium nanofibers of Fig. 2 the inventive method impel.
The photoluminescence collection of illustrative plates of the prepared six side's mangaic acid yttrium nanofibers of Fig. 3 the inventive method.
Embodiment
Embodiment 1, earlier with citric acid (C
6H
8O
7) be dissolved in the deionized water that to form concentration be 0.3g/mL citric acid (C
6H
8O
7) solution; Again with Y (NO
3)
3, Mn (CH
3COO)
2Add to stir to clarify in the citric acid solution transparent, Y (NO wherein
3)
36H
2O: Mn (CH
3COO)
24H
2O: C
6H
8O
7Mol ratio=1: 1: 2; Solution left standstill is placed and to be placed it in after 48 hours in the water-bath in 60 ℃ of heated and stirred 6 hours, adds molecular weight and be 1.3 * 106 polyvinylpyrrolidone (PVP) in solution, continues to be stirred to PVP and dissolves fully, makes the concentration of PVP remain on 0.03g/mL; This high polymeric solution being added to internal diameter at last is 2mm, syringe needle is in the plastic injector of stainless steel syringe needle, and syringe is added in the syringe pump, and it is 0.3mL/h that the startup syringe pump makes the injection flow velocity, open high-voltage power supply simultaneously and provide the voltage of 20kV, collect fiber with monocrystalline silicon piece to syringe needle; Place loft drier to put into retort furnace after 8 hours the fiber of collecting and be warming up to 1400 ℃, and, obtain six side's mangaic acid yttrium nanofibers in insulation calcining 6 hours with the heat-up rate of 1 ℃/min 100 ℃ of dryings.
Embodiment 2, earlier with citric acid (C
6H
8O
7) be dissolved in the deionized water that to form concentration be 0.2g/mL citric acid (C
6H
8O
7) solution; Again with Y (NO
3)
3, Mn (CH
3COO)
2Add to stir to clarify in the citric acid solution transparent, Y (NO wherein
3)
36H
2O: Mn (CH
3COO)
24H
2O: C
6H
8O
7Mol ratio=1: 1: 2; Solution left standstill is placed and to be placed it in after 24 hours in the water-bath in 50 ℃ of heated and stirred 7 hours, adds molecular weight and be 1.3 * 106 polyvinylpyrrolidone (PVP) in solution, continues to be stirred to PVP and dissolves fully, makes the concentration of PVP remain on 0.02g/mL; This high polymeric solution being added to internal diameter at last is 1mm, syringe needle is in the plastic injector of stainless steel syringe needle, and syringe is added in the syringe pump, and it is 0.4mL/h that the startup syringe pump makes the injection flow velocity, open high-voltage power supply simultaneously and provide the voltage of 25kV, collect fiber with monocrystalline silicon piece to syringe needle.Place loft drier to put into retort furnace after 7 hours the fiber of collecting and be warming up to 1200 ℃, and, obtain six side's mangaic acid yttrium nanofibers in insulation calcining 8 hours with the heat-up rate of 3 ℃/min 120 ℃ of dryings.
Embodiment 3, earlier with citric acid (C
6H
8O
7) be dissolved in the deionized water that to form concentration be 0.4g/mL citric acid (C
6H
8O
7) solution; Again with Y (NO
3)
3, Mn (CH
3COO)
2Add to stir to clarify in the citric acid solution transparent, Y (NO wherein
3)
36H
2O: Mn (CH
3COO)
24H
2O: C
6H
8O
7Mol ratio=1: 1: 2; Solution left standstill is placed and to be placed it in after 36 hours in the water-bath in 80 ℃ of heated and stirred 4 hours, adds molecular weight and be 1.3 * 106 polyvinylpyrrolidone (PVP) in solution, continues to be stirred to PVP and dissolves fully, makes the concentration of PVP remain on 0.04g/mL; This high polymeric solution being added to internal diameter at last is 2mm, syringe needle is in the plastic injector of stainless steel syringe needle, and syringe is added in the syringe pump, and it is 0.6mL/h that the startup syringe pump makes the injection flow velocity, open high-voltage power supply simultaneously and provide the voltage of 25kV, collect fiber with monocrystalline silicon piece to syringe needle.Place loft drier to put into retort furnace after 6 hours the fiber of collecting and be warming up to 1100 ℃, and, obtain six side's mangaic acid yttrium nanofibers in insulation calcining 10 hours with the heat-up rate of 4 ℃/min 140 ℃ of dryings.
Embodiment 4, earlier with citric acid (C
6H
8O
7) be dissolved in the deionized water that to form concentration be 0.3g/mL citric acid (C
6H
8O
7) solution; Again with Y (NO
3)
3, Mn (CH
3COO)
2Add to stir to clarify in the citric acid solution transparent, Y (NO wherein
3)
36H
2O: Mn (CH
3COO)
24H
2O: C
6H
8O
7Mol ratio=1: 1: 2; Solution left standstill is placed and to be placed it in after 72 hours in the water-bath in 90 ℃ of heated and stirred 3 hours, adds molecular weight and be 1.3 * 106 polyvinylpyrrolidone (PVP) in solution, continues to be stirred to PVP and dissolves fully, makes the concentration of PVP remain on 0.05g/mL; This high polymeric solution being added to internal diameter at last is 3mm, syringe needle is in the plastic injector of stainless steel syringe needle, and syringe is added in the syringe pump, and it is 0.7mL/h that the startup syringe pump makes the injection flow velocity, open high-voltage power supply simultaneously and provide the voltage of 30kV, collect fiber with monocrystalline silicon piece to syringe needle.Place loft drier to put into retort furnace after 4 hours the fiber of collecting and be warming up to 1000 ℃, and, obtain six side's mangaic acid yttrium nanofibers in insulation calcining 12 hours with the heat-up rate of 5 ℃/min 150 ℃ of dryings.
As can see from Figure 1, six side's mangaic acid yttrium nanofibers of embodiment 1~4 preparation are pure phases, calculate half-peak width according to the Scherrer formula simultaneously and can find that material is a nanometer scale.
As can see from Figure 2, embodiment 1~4 prepared six side's mangaic acid yttrium nanofibers, tropeolin-D is decomposed much in the photocatalysis performance.
As can see from Figure 3, the photoluminescence collection of illustrative plates of embodiment 1~4 prepared six side's mangaic acid yttrium nanofibers, along with soaking time increases, the photoluminescence spectrum of material reduces on the contrary.
In a word, nanofiber of the present invention has good magneto-electric coupled performance, and this nanofiber does not contain any volatile element, preparation is simple for fiber simultaneously, therefore the method for preparation six many iron of side's mangaic acid yttrium property nanofibers is fit to industrialization promotion and scale operation among the present invention, has broad application prospects on many iron sexual function material.