CN112876244A - Strontium zirconate inorganic fiber and preparation method thereof - Google Patents
Strontium zirconate inorganic fiber and preparation method thereof Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/6225—Fibres based on zirconium oxide, e.g. zirconates such as PZT
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3213—Strontium oxides or oxide-forming salts thereof
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Abstract
The invention relates to strontium zirconate inorganic fiber and a preparation method thereof. The preparation method comprises the steps of heating and dissolving a zirconium source, a strontium source, an organic ligand and a spinning aid in a water solution according to a certain proportion to prepare strontium zirconate precursor sol; obtaining strontium zirconate precursor fiber by using a strontium zirconate precursor sol through an electrostatic spinning method; and carrying out heat treatment on the strontium zirconate precursor fiber to prepare the strontium zirconate inorganic fiber. The obtained sol is stable and reliable, good in spinnability, easy to prepare by spinning, high in solid content of precursor fiber, and the diameter of the prepared strontium zirconate inorganic fiber is 0.5-1.0 mu m, and the fiber form is kept stable under the high temperature condition of room temperature to 1400 ℃.
Description
Technical Field
The invention relates to a strontium zirconate inorganic fiber and a preparation method thereof, belonging to the field of inorganic non-metallic materials.
Background
In recent years, with the long-term operation requirement of high-temperature kilns and the improvement of the national emission standards of energy conservation and environmental protection, a heat insulation system represented by a high-temperature energy-saving kiln heat insulation layer puts higher requirements on high-temperature-resistant, low-thermal-conductivity and high-strength heat insulation materials so as to solve the problems of insufficient high-temperature crystallization, phase change, temperature resistance and the like of the traditional inorganic fibers. Therefore, the development of inorganic fibers having excellent heat insulating properties such as high melting point and low thermal conductivity has become one of the needs for the research of advanced heat insulating systems.
Strontium zirconate (SrZrO)3) Is a perovskite type structural material, has high melting point (2800 ℃), low thermal conductivity (-2.1W/(m.K)), and high thermal expansion coefficient (10.9 multiplied by 10)-6 K-1) And good sintering resistance activity, and the like, and is a promising thermal barrier coating material and a high-grade thermal insulation material. The excellent thermophysical properties of the strontium zirconate itself are combined with the one-dimensional fiber structure, so that the advantages of the strontium zirconate and the fiber structure on the high-temperature heat-insulating property can be more fully exerted, and the strontium zirconate is a promising high-temperature inorganic fiber heat-insulating material. However, no report on strontium zirconate fibers has been found so far. The invention is provided for making up the deficiencies of the research of the strontium zirconate fiber.
Disclosure of Invention
In order to solve the problem of the lack of research on strontium zirconate fibers, the invention provides the strontium zirconate inorganic fiber and the preparation method thereof, provides a new morphological structure for the application of strontium zirconate materials, and provides a new product for the high-temperature heat insulation application of strontium zirconate.
The molecular formula of the strontium zirconate inorganic fiber prepared by the invention is SrZrO3The fiber diameter is 0.5-1.0 μm, and the fiber shape is kept stable under the condition of high temperature of room temperature to 1400 ℃.
The technical scheme of the invention is as follows:
a preparation method of strontium zirconate inorganic fiber comprises the following steps:
(a) preparation of strontium zirconate precursor sol
Adding raw materials of zirconium oxychloride and an organic ligand into water with a mass ratio of solid to water =0.5:5 according to a molar ratio of zirconium oxychloride to organic ligand =1: 0.1-2.5, and dissolving to obtain a zirconium oxide precursor sol; under the condition of heating and stirring at the temperature of 20-85 ℃, adding a strontium source with the molar ratio of Zr to Sr =1 to 1 into the zirconia precursor sol, and dissolving to prepare strontium zirconate sol; adding a high molecular polymer with the mass fraction of 0.05-12% into the strontium zirconate sol, and fully dissolving to obtain a strontium zirconate precursor sol;
(b) preparation of strontium zirconate precursor fiber by electrostatic spinning method
Preparing strontium zirconate precursor fiber from the strontium zirconate precursor sol obtained in the step (a) through electrostatic spinning, wherein the electrostatic spinning process conditions are that the spinning distance is 6-28 cm, the spinning voltage is 6-50 kV, the sol propelling speed is 0.4-4.0 mL/h, the ambient temperature is 10-35 ℃, and the ambient humidity is 10-55%;
(c) preparation of strontium zirconate inorganic fiber
Heating the strontium zirconate precursor fiber obtained in the step (b) to 450-600 ℃ at a heating rate of 0.5-5 ℃/min under the atmosphere condition, and preserving the heat for 0-3 h; and then heating to 800-1200 ℃ at the heating rate of 0.5-10 ℃/min, and preserving the heat for 1-5 h to prepare the strontium zirconate inorganic fiber.
Preferably, when the organic ligand is acetic acid, the zirconium oxychloride of step (a) has an organic ligand =1: 1.0-1.5; when the organic ligand is ethylene glycol, the ratio of the zirconium oxychloride to the organic ligand =1: 0.5-1.0; when the organic ligand is acetylacetone or ethyl acetoacetate, the ratio of zirconium oxychloride to organic ligand =1: 0.8-1.0 in step (a).
According to the invention, the mass ratio of the solid to the water in the step (a) is preferably =1 (1.5-2).
According to the invention, the heating temperature in the step (a) is preferably 45-60 ℃.
Preferably according to the present invention, when the organic ligand is acetic acid, the strontium source of step (a) is strontium oxide, strontium hydroxide, strontium carbonate or strontium bicarbonate; when the organic ligand is ethylene glycol, acetylacetone or ethyl acetoacetate, the strontium source of Zr: Sr =1:1 in the step (a) is a mixture of strontium oxide, strontium hydroxide, strontium carbonate or strontium bicarbonate of Zr: Sr =1 (0.6-0.8) and strontium acetate or strontium nitrate of Zr: Sr =1 (0.2-0.4).
According to the invention, when the high molecular polymer in the step (a) is polyethylene oxide, the addition amount of the high molecular polymer is 0.2-1.5% of the mass fraction of the solution; when the high molecular polymer in the step (a) is polyvinylpyrrolidone, the addition amount of the high molecular polymer is 3-8% of the mass fraction of the solution; when the high molecular polymer in the step (a) is one or a combination of polymethyl methacrylate and polyvinyl alcohol, the addition amount of the high molecular polymer is 4-12% of the mass fraction of the solution.
Preferably according to the present invention, the electrospinning process conditions in step (b) are: the spinning distance is 12-28 cm, the spinning voltage is 12-30 kV, the sol propelling speed is 0.6-2.0 mL/h, the ambient temperature is 20-30 ℃, and the ambient humidity is 10-45%.
Preferably, according to the present invention, the atmosphere in step (c) is an air atmosphere.
Preferably, according to the invention, the heat treatment system in the step (c) is that the strontium zirconate precursor fiber is heated to 450 ℃ at the heating rate of 1 ℃/min under the air condition; and then heating to 800-1200 ℃ at the heating rate of 2 ℃/min, and preserving the heat for 2h to obtain the strontium zirconate inorganic fiber.
The invention obtains the following excellent effects:
1. the invention has simple process, wide raw material source, low cost, stable sol, easy spinning and mass preparation.
2. The strontium zirconate fiber prepared by the invention has the fiber diameter of 0.5-1.0 μm, and keeps stable fiber shape under the high temperature condition of room temperature to 1400 ℃.
3. The strontium zirconate inorganic fiber prepared by the invention is a novel perovskite type zirconium-based oxide fiber material, and has wide application prospect in the field of high-temperature heat insulation and preservation.
Drawings
FIG. 1 is a strontium zirconate precursor fiber prepared in example 1.
FIG. 2 is an XRD pattern of strontium zirconate fiber obtained in example 1 heat-treated to 1200 ℃.
FIG. 3 is an XRD pattern of strontium zirconate fiber obtained in example 4 heat-treated to 1200 ℃.
FIG. 4 is an SEM photograph of strontium zirconate fibers obtained in example 4 heat-treated to 1200 ℃.
Detailed Description
The present invention will be further described by way of examples, but not limited thereto, with reference to the accompanying drawings.
The raw materials used in the examples are all commercially available raw materials.
Example 1:
a preparation method of strontium zirconate inorganic fiber comprises the following steps:
(a) preparation of strontium zirconate precursor sol
Adding raw materials of zirconium oxychloride and glacial acetic acid into water with a mass ratio of solid to water of =1:2 according to a molar ratio of zirconium oxychloride to glacial acetic acid of =1: 1.2, and dissolving to obtain a zirconium oxide precursor sol; under the condition of heating and stirring at 60 ℃, adding strontium carbonate with the molar ratio of Zr to Sr =1 to 1 into the zirconia precursor sol, and dissolving to prepare strontium zirconate sol; adding polyoxyethylene with the mass fraction of 1.5% into the strontium zirconate sol, and fully dissolving to prepare strontium zirconate precursor sol;
(b) preparation of strontium zirconate precursor fiber by electrostatic spinning method
And (b) preparing the strontium zirconate precursor fiber from the strontium zirconate precursor sol obtained in the step (a) through electrostatic spinning, wherein the electrostatic spinning process conditions are that the spinning distance is 16cm, the spinning voltage is 16kV, the sol propelling speed is 2.0mL/h, the ambient temperature is 10-25 ℃, the ambient humidity is 20-35%, and the prepared strontium zirconate precursor fiber is shown in figure 1.
(c) Preparation of strontium zirconate inorganic fiber
Heating the strontium zirconate precursor fiber obtained in the step (b) to 450 ℃ at a heating rate of 1 ℃/min under the atmosphere condition; then heating to 1200 ℃ at the heating rate of 2 ℃/min, and preserving the heat for 2h to prepare the strontium zirconate inorganic fiber. The XRD (X-ray diffraction) pattern of the crystal phase test result of the prepared strontium zirconate fiber is shown in figure 1, the SEM (scanning electron microscope) result of the fiber morphology is shown in figure 2, and the diameter distribution of the fiber is 0.5-1.0 mu m.
Example 2:
as described in example 1, except that strontium carbonate in step (a) was replaced with strontium oxide.
Example 3:
as described in example 1, except that the strontium carbonate in step (a) was replaced with strontium hydroxide.
Example 4:
as described in example 1, except that step (a), the specific step (a) is carried out as follows: adding raw materials of zirconium oxychloride and acetylacetone into water with a mass ratio of solid to water =1:1.5 according to a molar ratio of zirconium oxychloride to acetylacetone =1:1, and dissolving to obtain a zirconium oxide precursor sol; under the condition of heating and stirring at 50 ℃, adding strontium carbonate with the molar ratio of Zr to Sr =1: 0.8 into the zirconia precursor sol, and adding strontium nitrate with the molar ratio of Zr to Sr =1: 0.2 after dissolving to prepare strontium zirconate sol; and adding polyoxyethylene with the mass fraction of 2% into the strontium zirconate sol, and fully dissolving to obtain the strontium zirconate precursor sol. The XRD (X-ray diffraction) pattern of the crystal phase test result of the prepared strontium zirconate fiber is shown in figure 3, the SEM (scanning electron microscope) result of the fiber morphology is shown in figure 4, and the diameter distribution of the fiber is 0.5-1.0 mu m.
Example 5:
as described in example 4, except that the acetylacetone in step (a) was replaced with ethylene glycol.
Example 6:
as described in example 4, except that the strontium nitrate in step (a) was changed to strontium chloride.
Claims (7)
1. The strontium zirconate inorganic fiber is characterized in that the molecular formula of the strontium zirconate inorganic fiber is SrZrO3The fiber diameter is 0.5-1.0 μm, and the fiber shape is kept intact under the condition of high temperature of room temperature to 1400 ℃.
2. The method for preparing the strontium zirconate inorganic fiber according to claim 1, comprising the following steps:
(a) preparation of strontium zirconate precursor sol
Adding raw materials of zirconium oxychloride and an organic ligand into water with a mass ratio of solid to water =0.5:5 according to a molar ratio of zirconium oxychloride to organic ligand =1: 0.1-2.5, and dissolving to obtain a zirconium oxide precursor sol; under the condition of heating and stirring at the temperature of 20-85 ℃, adding a strontium source with the molar ratio of Zr to Sr =1 to 1 into the zirconia precursor sol, and dissolving to prepare strontium zirconate sol; adding a high molecular polymer with the mass fraction of 0.05-12% into the strontium zirconate sol, and fully dissolving to obtain a strontium zirconate precursor sol;
(b) preparation of strontium zirconate precursor fiber by electrostatic spinning method
Preparing strontium zirconate precursor fiber from the strontium zirconate precursor sol obtained in the step (a) through electrostatic spinning, wherein the electrostatic spinning process conditions are that the spinning distance is 6-28 cm, the spinning voltage is 6-50 kV, the sol propelling speed is 0.4-4.0 mL/h, the ambient temperature is 10-35 ℃, and the ambient humidity is 10-55%;
(c) preparation of strontium zirconate inorganic fiber
Heating the strontium zirconate precursor fiber obtained in the step (b) to 450-600 ℃ at a heating rate of 0.5-5 ℃/min under the atmosphere condition, and preserving the heat for 0-3 h; and then heating to 800-1200 ℃ at the heating rate of 0.5-10 ℃/min, and preserving the heat for 1-5 h to prepare the strontium zirconate inorganic fiber.
3. The method of claim 2, wherein the organic ligand of step (a) is one of acetic acid, ethylene glycol, acetylacetone, ethyl acetoacetate, or a combination thereof.
4. The method of preparing strontium zirconate inorganic fiber according to claim 2, wherein when the organic ligand is acetic acid, the zirconium oxychloride of step (a) has an organic ligand =1: 0.8-2.5; when the organic ligand is ethylene glycol, the ratio of the zirconium oxychloride to the organic ligand =1: 0.1-1.2; when the organic ligand is acetylacetone or ethyl acetoacetate, the ratio of zirconium oxychloride to organic ligand =1: 0.8-1.2 in step (a).
5. The method of claim 2, wherein the strontium source in the step (a) is one of strontium acetate, strontium hydroxide, strontium oxide, strontium nitrate, strontium carbonate, strontium bicarbonate, strontium chloride, or a combination thereof.
6. The method of claim 2, wherein the polymer in step (a) is one of polyvinylpyrrolidone, polyethylene oxide, polymethyl methacrylate, polyvinyl alcohol, or a combination thereof.
7. The method of preparing strontium zirconate inorganic fiber according to claim 2, wherein the atmosphere in step (c) is one of air, water vapor, nitrogen or a combination thereof.
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| CN101407337A (en) * | 2008-11-07 | 2009-04-15 | 天津工业大学 | Method of preparing perovskite type zirconate hollow nano material |
| CN103993387A (en) * | 2014-05-30 | 2014-08-20 | 山东大学 | Method for preparing ultrahigh-temperature-resistant kilometric continuous zirconia crystal fiber |
| KR20150015856A (en) * | 2013-08-01 | 2015-02-11 | 주식회사 엘지화학 | Fiber structure body, anode comprising the same, manufacturing method of the same |
| CN106929947A (en) * | 2015-12-30 | 2017-07-07 | 山东大学 | The preparation method of poly-vinegar acid oxygen zirconium precursor body colloidal sol spinning solution and sub-micron zirconium oxide crystal fibre |
| CN110170282A (en) * | 2019-05-07 | 2019-08-27 | 清华大学 | A kind of anisotropy stratiform inorfil aerogel material and preparation method thereof |
| CN110330333A (en) * | 2019-07-23 | 2019-10-15 | 安徽钛谷纳米材料有限公司 | A method of preparing nanoscale yttrium stable zirconium oxide composite granule |
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- 2021-04-08 CN CN202110376425.2A patent/CN112876244B/en active Active
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| CN101407337A (en) * | 2008-11-07 | 2009-04-15 | 天津工业大学 | Method of preparing perovskite type zirconate hollow nano material |
| KR20150015856A (en) * | 2013-08-01 | 2015-02-11 | 주식회사 엘지화학 | Fiber structure body, anode comprising the same, manufacturing method of the same |
| CN103993387A (en) * | 2014-05-30 | 2014-08-20 | 山东大学 | Method for preparing ultrahigh-temperature-resistant kilometric continuous zirconia crystal fiber |
| CN106929947A (en) * | 2015-12-30 | 2017-07-07 | 山东大学 | The preparation method of poly-vinegar acid oxygen zirconium precursor body colloidal sol spinning solution and sub-micron zirconium oxide crystal fibre |
| CN110170282A (en) * | 2019-05-07 | 2019-08-27 | 清华大学 | A kind of anisotropy stratiform inorfil aerogel material and preparation method thereof |
| CN110330333A (en) * | 2019-07-23 | 2019-10-15 | 安徽钛谷纳米材料有限公司 | A method of preparing nanoscale yttrium stable zirconium oxide composite granule |
Non-Patent Citations (2)
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| R.C.PULLAR ET AL.: ""Blow spun strontium zirconate fibres produced from a sol-gel precursor"", 《JOURNAL OF MATERIALS SCIENCE》 * |
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