CN102775148A - Preparation method of magnesium diboride ceramic fiber precursor electrostatic spinning solution - Google Patents
Preparation method of magnesium diboride ceramic fiber precursor electrostatic spinning solution Download PDFInfo
- Publication number
- CN102775148A CN102775148A CN2012102415700A CN201210241570A CN102775148A CN 102775148 A CN102775148 A CN 102775148A CN 2012102415700 A CN2012102415700 A CN 2012102415700A CN 201210241570 A CN201210241570 A CN 201210241570A CN 102775148 A CN102775148 A CN 102775148A
- Authority
- CN
- China
- Prior art keywords
- magnesium
- electrostatic spinning
- containing compound
- preparation
- ceramic fiber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention relates to a preparation method of a magnesium diboride ceramic fiber precursor electrostatic spinning solution, which comprises the following steps: (1) dissolving a magnesium-containing compound in ethanol, and adding a surfactant to obtain an ethanol solution of magnesium-containing compound; dissolving sodium borohydride in ethanol, and adding a surfactant to obtain an ethanol solution of sodium borohydride; while stirring, slowly and dropwisely adding the ethanol solution of sodium borohydride into the ethanol solution of magnesium-containing compound until the reaction is complete, carrying out ultrasonic treatment for 1-20 minutes, standing, and filtering out the precipitate to obtain a precursor solution; and (2) at room temperature, evenly mixing the precursor solution and spinning aids, and concentrating to obtain the magnesium diboride fiber precursor electrostatic spinning solution. The invention has the advantages of simple operating technique, low cost and low requirements for equipment; and the prepared spinning solution has favorable spinnability.
Description
Technical field
The invention belongs to the preparation field of superconductor fibre presoma electrostatic spinning liquid, particularly a kind of preparation method of magnesium diboride ceramic fiber presoma electrostatic spinning liquid.
Background technology
Along with high-tech and industrialized development, military, civilian etc. all higher stricter requirement has been proposed for the performance and the cost of superconducting material.Magnesium diboride (MgB
2) critical temperature of superconducting material is 39K, is lower than high temperature superconducting materia.But MgB
2Have simple binary chemical constitution and hexagonal crystallographic texture, do not have complicated interface problem, crystal boundary does not have weak connection, has very high critical current density jc (～10
7A/cm
2) and high upper critical field H
C2, and raw-material cost is lower, and technology of preparing is easy to be more many than high temperature superconducting materia, so it all has good application in many aspects.
Though magnesium diboride has good performance, to fail at present to be widely used, major cause is the preparation method.The starting material and the technology of preparing of domestic and international powder for magnesium diboride, film, fiber all have research to a certain degree.Present MgB
2The preparation of wire rod and strip material mainly contains powder tubulature technology (P IT) and CTFF technology and CVD technology; Main all is to be obtained by independent magnesium and boron reaction; Can only make the fiber of hundreds of rice at most; And can't obtain uniform magnesium diboride fiber, the application of sol-gel technology then is expected to solve the problem of serialization.
Manashi Nath and B.A.Parkinson (Advanced Materials, 2006, be raw material 18:1865-1868) with magnesium bromide and Peng Qinghuana, adopt sol-gel method to prepare the magnesium diboride nanofiber; Feng Qingrong etc. (A sol-gel method for growing superconducting MgB2films.Supercond.Sci.Technol, 2011,24:15002-15006.) adopt sol-gel method to prepare the magnesium diboride film.
But also there is not relevant electrostatic spinning to prepare the research of magnesium diboride fiber both at home and abroad.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of magnesium diboride ceramic fiber presoma electrostatic spinning liquid, and this method is simple to operate, and is with low cost, low for equipment requirements; Prepared spinning solution good spinning property.
The preparation method of a kind of magnesium diboride ceramic fiber presoma electrostatic spinning liquid of the present invention comprises:
(1) preparation of precursor solution:
Magnesium-containing compound is dissolved in the ethanol, adds tensio-active agent again, obtain the ethanolic soln of magnesium-containing compound; Peng Qinghuana is dissolved in the ethanol, adds tensio-active agent again, obtain the ethanolic soln of Peng Qinghuana; Under agitation the ethanolic soln with above-mentioned Peng Qinghuana slowly is added drop-wise in the ethanolic soln of magnesium-containing compound, treats after the complete reaction supersound process 1 ~ 20 minute, leaves standstill after-filtration and falls deposition, obtains precursor solution;
(2) magnesium diboride ceramic fiber presoma electrostatic spinning liquid is synthetic:
Under the room temperature,, after concentrating, can obtain magnesium diboride fiber presoma electrostatic spinning liquid with above-mentioned precursor solution and spin finish aid uniform mixing.
Magnesium-containing compound described in the step (1) is a kind of in Magnesium Chloride Anhydrous, anhydrous magnesium bromide, the anhydrous magnesium iodide.
Tensio-active agent described in the step (1) is cetyl trimethylammonium bromide or X 2073.
The mol ratio of surfactant content sum and magnesium-containing compound is 1:1 ~ 1:50 in the ethanolic soln of the magnesium-containing compound described in the step (1) and the ethanolic soln of Peng Qinghuana.
The mol ratio of magnesium-containing compound described in the step (1) and Peng Qinghuana is 1:1 ~ 1:10.
Spin finish aid described in the step (2) is a kind of in Vinylpyrrolidone polymer, Z 150PH, polyoxyethylene glycol, polyoxyethylene, the hydroxypropylcellulose.
Spin finish aid described in the step (2) accounts for 10 ~ 40% of magnesium-containing compound, Peng Qinghuana, tensio-active agent (tensio-active agent sum in the ethanolic soln of magnesium-containing compound and the ethanolic soln of Peng Qinghuana) and spin finish aid total mass.
Know-why of the present invention: with ethanol, anhydrous magnesium-containing compound, Peng Qinghuana is main raw material, adds proper amount of surfactant, and improves the spinning property of spinning solution through adding the polymer spin finish aid, obtains stable spinning solution.
Beneficial effect:
(1) operating procedure of the present invention is simple, and is with low cost, lower to equipment requirements;
(2) the spinning solution good spinning property that obtains of the present invention has a extensive future.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The ethanolic soln that preparation contains the ethanolic soln of 0.1638g Peng Qinghuana and contains the 0.2291g magnesium chloride; In above-mentioned two solution, add the 0.0191g cetyl trimethylammonium bromide respectively; Fully after the dissolving ethanol solution of sodium borohydride slowly is added drop-wise in the middle of the magnesium chloride ethanolic soln, ultrasonication is 10 minutes after the stirring reaction, through leaving standstill fully; Get rid of deposition, obtain clarifying precursor solution; In solution, add the 0.1253g Vinylpyrrolidone polymer then, fully dissolving obtains uniform and stable magnesium diboride presoma electrostatic spinning solution after concentrating.
Embodiment 2
The ethanolic soln that preparation contains the ethanolic soln of 0.1638g Peng Qinghuana and contains the 0.1873g magnesium chloride; In above-mentioned two solution, add the 0.0151g cetyl trimethylammonium bromide respectively; Fully after the dissolving ethanol solution of sodium borohydride slowly is added drop-wise in the middle of the magnesium chloride ethanolic soln, ultrasonication is ten minutes after the stirring reaction, through leaving standstill fully; Get rid of deposition, obtain clarifying precursor solution; In solution, add the 0.1g Vinylpyrrolidone polymer then, fully dissolving obtains uniform and stable magnesium diboride presoma electrostatic spinning solution after concentrating.
Embodiment 3
The ethanolic soln that preparation contains the ethanolic soln of 0.1638g Peng Qinghuana and contains the 0.2063g magnesium chloride; In above-mentioned two solution, add the 0.015g cetyl trimethylammonium bromide respectively; Fully after the dissolving ethanol solution of sodium borohydride slowly is added drop-wise in the middle of the magnesium chloride ethanolic soln, ultrasonication is 15 minutes after the stirring reaction, through leaving standstill fully; Get rid of deposition, obtain clarifying precursor solution; In solution, add the 0.125g polyoxyethylene glycol, fully dissolving obtains uniform and stable magnesium diboride presoma electrostatic spinning solution after concentrating.
Embodiment 4
The ethanolic soln that preparation contains the ethanolic soln of 0.1638g Peng Qinghuana and contains the 0.2063g magnesium chloride; In above-mentioned two solution, add the 0.0142g X 2073 respectively; Fully after the dissolving ethanol solution of sodium borohydride slowly is added drop-wise in the middle of the magnesium chloride ethanolic soln, ultrasonication is after 15 minutes, through leaving standstill fully after the stirring reaction; Get rid of deposition, obtain clarifying precursor solution; In solution, add the 0.125g polyoxyethylene glycol, fully dissolving obtains uniform and stable magnesium diboride presoma electrostatic spinning solution after concentrating.
Embodiment 5
The ethanolic soln that preparation contains the ethanolic soln of 0.1638g Peng Qinghuana and contains the 0.4196g magnesium bromide; In above-mentioned two solution, add the 0.019g cetyl trimethylammonium bromide respectively; Fully after the dissolving ethanol solution of sodium borohydride slowly is added drop-wise in the middle of the magnesium chloride ethanolic soln, ultrasonication is after 15 minutes, through leaving standstill fully after the stirring reaction; Get rid of deposition, obtain clarifying precursor solution; In solution, add the 0.1246g Vinylpyrrolidone polymer, fully dissolving obtains uniform and stable magnesium diboride presoma electrostatic spinning solution after concentrating.
Embodiment 6
The ethanolic soln that preparation contains the ethanolic soln of 0.1638g Peng Qinghuana and contains the 0.6514g magnesium iodide; In above-mentioned two solution, add the 0.019g cetyl trimethylammonium bromide respectively; Fully after the dissolving ethanol solution of sodium borohydride slowly is added drop-wise in the middle of the magnesium chloride ethanolic soln, ultrasonication is 15 minutes after the stirring reaction, through leaving standstill fully; Get rid of deposition, obtain clarifying precursor solution; In solution, add the 0.1238g Vinylpyrrolidone polymer, fully dissolving obtains uniform and stable magnesium diboride presoma electrostatic spinning solution after concentrating.
Claims (7)
1. the preparation method of a magnesium diboride ceramic fiber presoma electrostatic spinning liquid comprises:
(1) magnesium-containing compound is dissolved in the ethanol, adds tensio-active agent again, obtain the ethanolic soln of magnesium-containing compound; Peng Qinghuana is dissolved in the ethanol, adds tensio-active agent again, obtain the ethanolic soln of Peng Qinghuana; Under agitation the ethanolic soln with above-mentioned Peng Qinghuana slowly is added drop-wise in the ethanolic soln of magnesium-containing compound, treats after the complete reaction supersound process 1 ~ 20 minute, leaves standstill after-filtration and falls deposition, obtains precursor solution;
(2) under the room temperature,, promptly obtain magnesium diboride fiber presoma electrostatic spinning liquid after concentrating with above-mentioned precursor solution and spin finish aid uniform mixing.
2. the preparation method of a kind of magnesium diboride ceramic fiber presoma electrostatic spinning liquid according to claim 1 is characterized in that: the magnesium-containing compound described in the step (1) is a kind of in Magnesium Chloride Anhydrous, anhydrous magnesium bromide, the anhydrous magnesium iodide.
3. the preparation method of a kind of magnesium diboride ceramic fiber presoma electrostatic spinning liquid according to claim 1, it is characterized in that: the tensio-active agent described in the step (1) is cetyl trimethylammonium bromide or X 2073.
4. the preparation method of a kind of magnesium diboride ceramic fiber presoma electrostatic spinning liquid according to claim 1 is characterized in that: the mol ratio of the content sum of tensio-active agent and magnesium-containing compound is 1:1 ~ 1:50 in the ethanolic soln of the magnesium-containing compound described in the step (1) and the ethanolic soln of Peng Qinghuana.
5. the preparation method of a kind of magnesium diboride ceramic fiber presoma electrostatic spinning liquid according to claim 1, it is characterized in that: the mol ratio of magnesium-containing compound described in the step (1) and Peng Qinghuana is 1:1 ~ 1:10.
6. the preparation method of a kind of magnesium diboride ceramic fiber presoma electrostatic spinning liquid according to claim 1 is characterized in that: the spin finish aid described in the step (2) is a kind of in Vinylpyrrolidone polymer, Z 150PH, polyoxyethylene glycol, polyoxyethylene, the hydroxypropylcellulose.
7. the preparation method of a kind of magnesium diboride ceramic fiber presoma electrostatic spinning liquid according to claim 1, it is characterized in that: the spin finish aid described in the step (2) accounts for 10 ~ 40% of magnesium-containing compound, Peng Qinghuana, tensio-active agent and spin finish aid total mass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102415700A CN102775148A (en) | 2012-07-12 | 2012-07-12 | Preparation method of magnesium diboride ceramic fiber precursor electrostatic spinning solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102415700A CN102775148A (en) | 2012-07-12 | 2012-07-12 | Preparation method of magnesium diboride ceramic fiber precursor electrostatic spinning solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102775148A true CN102775148A (en) | 2012-11-14 |
Family
ID=47120286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012102415700A Pending CN102775148A (en) | 2012-07-12 | 2012-07-12 | Preparation method of magnesium diboride ceramic fiber precursor electrostatic spinning solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102775148A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114990722A (en) * | 2022-06-21 | 2022-09-02 | 陕西师范大学 | Montmorillonite/magnesium diboride/polyvinyl alcohol composite flame-retardant fiber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880917A (en) * | 2010-02-05 | 2010-11-10 | 西安理工大学 | Method for preparing nano ceramic fibers |
| CN102108567A (en) * | 2009-12-25 | 2011-06-29 | 郭玉英 | Method for preparing superfine magnesia ceramic fibers |
| CN102351539A (en) * | 2011-07-05 | 2012-02-15 | 东华大学 | Method for preparing electrostatic spinning liquid of zirconium boride nano ceramic fiber |
-
2012
- 2012-07-12 CN CN2012102415700A patent/CN102775148A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102108567A (en) * | 2009-12-25 | 2011-06-29 | 郭玉英 | Method for preparing superfine magnesia ceramic fibers |
| CN101880917A (en) * | 2010-02-05 | 2010-11-10 | 西安理工大学 | Method for preparing nano ceramic fibers |
| CN101880917B (en) * | 2010-02-05 | 2011-11-16 | 西安理工大学 | Method for preparing nano ceramic fibers |
| CN102351539A (en) * | 2011-07-05 | 2012-02-15 | 东华大学 | Method for preparing electrostatic spinning liquid of zirconium boride nano ceramic fiber |
Non-Patent Citations (1)
| Title |
|---|
| MANASHI NATH 等: "A Simple Sol-Gel Synthesis of Superconducting MgB2 Nanowires", 《ADVANCED MATERIALS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114990722A (en) * | 2022-06-21 | 2022-09-02 | 陕西师范大学 | Montmorillonite/magnesium diboride/polyvinyl alcohol composite flame-retardant fiber |
| CN114990722B (en) * | 2022-06-21 | 2024-01-19 | 陕西师范大学 | Montmorillonite/magnesium diboride/polyvinyl alcohol composite flame-retardant fiber |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106469814B (en) | A kind of covering, negative electrode material, lithium ion battery and preparation method thereof | |
| CN101838934B (en) | Sizing agent for surface processing of glass fiber filter cloth and preparation method thereof | |
| CN109301204B (en) | Preparation method of hollow sphere structure tin sulfide/tin oxide lithium ion battery anode material | |
| CN101944594B (en) | Lithium ferrous silicate anode material for high-performance lithium ion battery and preparation method thereof | |
| CN102881871A (en) | Method for preparing graphite/silicone composite material for negative electrode of lithium ion battery | |
| CN102503387B (en) | Method for preparing high-purity super-fine mullite powder | |
| CN105696325A (en) | Antifungal anti-mite textile material and preparation method thereof | |
| CN104659378B (en) | A kind of intermediate temperature solid oxide fuel cell nanofiber composite cathode preparation method | |
| CN105129805A (en) | Preparation method of silicon oxide/tin antimony oxide/zinc oxide ternary composite material | |
| CN109301194A (en) | Compound porous hard carbon material of phosphorus quantum dot and its preparation method and application | |
| CN101569479B (en) | Method for producing negative ion silk quilt | |
| CN102703977A (en) | Hydroxyapatite mono-crystal nano-rod and preparation method thereof | |
| CN106654188A (en) | Super-fine nanocrystal lithium vanadium phosphate positive electrode material and preparation method therefor | |
| CN103523819A (en) | Method for preparing monodisperse antimony-doped tin oxide nano-powder | |
| CN104167541B (en) | For the positive electrode preparation technology of sodium-ion battery | |
| CN104638228A (en) | Coaxial carbon-coated bunchy vanadium potassium phosphate nanowire, as well as preparation method and application of nanowire | |
| CN102775148A (en) | Preparation method of magnesium diboride ceramic fiber precursor electrostatic spinning solution | |
| CN105261485B (en) | A kind of preparation method of capacitor electrode material | |
| CN101295563B (en) | Production method of MgB2 block material doped with organic matter | |
| CN103833080B (en) | A kind of preparation method of molybdic acid cadmium porous ball | |
| CN102242407B (en) | Method for preparing silicon oxide/silver nano composite fibers | |
| CN106602065A (en) | Preparation method of self-assembled three-dimensional charcoal sodium-ion battery anode carbon material | |
| CN102642844A (en) | Lithium chloride molten salt method for preparing lanthanum silicate electrolyte material powder with oxidapatite structure | |
| CN107777718B (en) | A kind of Y2O3Nano-powder and preparation method thereof | |
| CN103165875B (en) | Lithium-ion pre-embedded vanadium pentoxide nanobelt as well as preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20121114 |