CN102079543A - Preparation method of hexagonal manganese acid yttrium nanofiber - Google Patents
Preparation method of hexagonal manganese acid yttrium nanofiber Download PDFInfo
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- CN102079543A CN102079543A CN 201110045005 CN201110045005A CN102079543A CN 102079543 A CN102079543 A CN 102079543A CN 201110045005 CN201110045005 CN 201110045005 CN 201110045005 A CN201110045005 A CN 201110045005A CN 102079543 A CN102079543 A CN 102079543A
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Abstract
The invention discloses a preparation method of hexagonal manganese acid yttrium nanofiber, which is used for solving the technical problem of large granularity of manganese acid yttrium materials prepared by using the traditional preparation method. The invention has the following technical schemes: dissolving citric acid into deionized water to form a citric acid solution; adding Y(NO3)3 and Mn(CH3COO)2 into the citric acid solution to stir until the solution is clear and transparent; standing the solution and putting into a water bath pot for heating and stirring; adding polyvinylpyrrolidone into the solution and continuously stirring until the polyvinylpyrrolidone is completely dissolved, and keeping the concentration of the polyvinylpyrrolidone; carrying out electrostatic spinning by using an injection pump and a high-voltage power source; collecting fibers by using a monocrystalline silicon wafer; and putting the collected fibers into a drying box for drying and then putting into a muffle furnace for keeping the temperature and forging to obtain hexagonal manganese acid yttrium nanofiber.
Description
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.
Claims (1)
1. the preparation method of side's mangaic acid yttrium nanofiber is characterized in that 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.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102242407A (en) * | 2011-06-02 | 2011-11-16 | 西北工业大学 | Method for preparing silicon oxide/silver nano composite fibers |
| CN102874878A (en) * | 2012-09-17 | 2013-01-16 | 陕西科技大学 | Manganese acid yttrium nano powder preparation method according to microwave-hydrothermal method |
| CN102895968A (en) * | 2012-09-17 | 2013-01-30 | 陕西科技大学 | Preparation method of manganese oxide yttrium semiconductor photocatalytic powder |
| CN102910913A (en) * | 2012-09-26 | 2013-02-06 | 河南科技大学 | Preparation process of YMnO3 dielectric ceramic and YMnO3 dielectric ceramic capacitor |
| CN109972198A (en) * | 2019-05-13 | 2019-07-05 | 北京理工大学 | A kind of preparation method of sheet mangaic acid erbium monocrystalline |
| CN115784314A (en) * | 2022-11-28 | 2023-03-14 | 昆明理工大学 | Method for preparing strontium manganate with assistance of jet plasma |
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| CN1970142A (en) * | 2006-11-08 | 2007-05-30 | 中国科学技术大学 | Visible light responsive photocatalyst and its preparing process |
| CN101870498A (en) * | 2010-04-16 | 2010-10-27 | 北京工业大学 | Polyethylene glycol and citric acid auxiliary template method of three-dimensional ordered macroporous and chain LaMnO3 |
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2011
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102242407A (en) * | 2011-06-02 | 2011-11-16 | 西北工业大学 | Method for preparing silicon oxide/silver nano composite fibers |
| CN102242407B (en) * | 2011-06-02 | 2013-08-14 | 西北工业大学 | Method for preparing silicon oxide/silver nano composite fibers |
| CN102874878A (en) * | 2012-09-17 | 2013-01-16 | 陕西科技大学 | Manganese acid yttrium nano powder preparation method according to microwave-hydrothermal method |
| CN102895968A (en) * | 2012-09-17 | 2013-01-30 | 陕西科技大学 | Preparation method of manganese oxide yttrium semiconductor photocatalytic powder |
| CN102874878B (en) * | 2012-09-17 | 2014-06-04 | 陕西科技大学 | Manganese acid yttrium nano powder preparation method according to microwave-hydrothermal method |
| CN102910913A (en) * | 2012-09-26 | 2013-02-06 | 河南科技大学 | Preparation process of YMnO3 dielectric ceramic and YMnO3 dielectric ceramic capacitor |
| CN109972198A (en) * | 2019-05-13 | 2019-07-05 | 北京理工大学 | A kind of preparation method of sheet mangaic acid erbium monocrystalline |
| CN115784314A (en) * | 2022-11-28 | 2023-03-14 | 昆明理工大学 | Method for preparing strontium manganate with assistance of jet plasma |
| CN115784314B (en) * | 2022-11-28 | 2024-03-12 | 昆明理工大学 | Method for preparing strontium manganate with assistance of jet plasma |
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| CN102079543B (en) | 2012-07-04 |
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Owner name: JIANGSU WENFENG CHEMICAL FIBER GROUP CO., LTD. Free format text: FORMER OWNER: NORTHWESTERN POLYTECHNICAL UNIVERSITY Effective date: 20140814 Owner name: NORTHWESTERN POLYTECHNICAL UNIVERSITY Effective date: 20140814 |
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Effective date of registration: 20140814 Address after: 226600 No. 105 Changjiang West Road, Haian Town, Haian County, Nantong, Jiangsu Patentee after: Jiangsu Wenfeng Chemical Fiber Group Co., Ltd. Patentee after: Northwestern Polytechnical University Address before: 710072 Xi'an friendship West Road, Shaanxi, No. 127 Patentee before: Northwestern Polytechnical University |