CN113151932B - Preparation method and preparation material of yttrium silicate nanofiber - Google Patents

Preparation method and preparation material of yttrium silicate nanofiber Download PDF

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CN113151932B
CN113151932B CN202110469645.XA CN202110469645A CN113151932B CN 113151932 B CN113151932 B CN 113151932B CN 202110469645 A CN202110469645 A CN 202110469645A CN 113151932 B CN113151932 B CN 113151932B
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yttrium
yttrium silicate
spinning
fiber
prepared
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CN113151932A (en
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赵步月
黄海明
陈群教
李玮洁
王爽
黄杰
陈嘉龙
明四维
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Shandong Yuanrui Test Equipment Co ltd
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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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
    • C04B35/16—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 silicates other than clay
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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
    • C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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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
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract

The invention discloses a preparation method of yttrium silicate nanofiber and a preparation material thereof, belonging to the technical field of chemical material preparation methods, wherein a certain amount of catalytic liquid is dripped into tetraethoxysilane, and silica sol is obtained after stirring; adding an yttrium source into the silica sol, and stirring to obtain yttrium silica sol; adding a spinning auxiliary agent into yttrium silica sol to obtain yttrium silicate precursor spinning solution; performing electrostatic spinning on the yttrium silicate precursor spinning solution obtained in the step one to obtain yttrium silicate precursor fibers; and (4) carrying out high-temperature heat treatment on the yttrium silicate precursor fiber obtained in the step two in an air environment to obtain an yttrium silicate nanofiber material product. The yttrium silicate precursor spinning solution with good spinnability is prepared by adopting a sol-gel method, and the yttrium silicate nano-fiber with compact structure is prepared by an electrostatic spinning technology. The fiber prepared by the method overcomes the defect that other components are introduced in the preparation process, improves the purity of the product and ensures the quality of the product.

Description

Preparation method and preparation material of yttrium silicate nanofiber
Technical Field
The invention relates to a preparation method of yttrium silicate nanofibers and a preparation material thereof, belonging to the technical field of preparation methods of chemical materials.
Background
Yttrium silicate materials are one type of rare earth silicate, and the common three yttrium silicate crystal structures are Y 2 SiO 5 、Y 2 Si 2 O 7 And Y 4 Si 3 O 12 Silicic acid of the first two structuresYttrium is widely used because of its extremely high melting point. And due to the excellent crystal structure and physicochemical properties, the yttrium silicate material has a plurality of good characteristics, such as low thermal conductivity, low thermal expansion coefficient, low oxygen permeability, low volatility, good high-temperature stability, good high-temperature corrosion resistance, good mechanical properties and the like. Therefore, yttrium silicate materials are used as high-performance ceramics, high-temperature oxidation-resistant coatings, optical matrix materials, dielectric materials, and the like.
Chinese patent literature, application publication number is: CN102817094A discloses a method for preparing europium-doped yttrium disilicate red luminescent nano-fibers, which comprises weighing a certain amount of yttrium oxide Y 2 O 3 And europium oxide Eu 2 O 3 The molar ratio of the two is 95: 5, namely the molar percentage of europium ions is 5 percent, and dilute nitric acid HNO is used 3 Dissolving and evaporating to obtain Y (NO) 3 ) 3 And Eu (NO) 3 ) 3 Mixing the crystals, adding tetraethoxysilane Si (C) 2 H 5 O) 4 Let Y be 3+ Adding Eu 3+ With Si (C) 2 H 5 O) 4 Adding a proper amount of N, N-dimethylformamide DMF solvent and polyvinylpyrrolidone PVP (polyvinylpyrrolidone), magnetically stirring at room temperature for 4 hours, standing for 2 hours to form spinning solution, and carrying out electrostatic spinning and air heat treatment to obtain the europium-doped yttrium disilicate red luminescent nanofiber. However, a large amount of nitric acid is used in the preparation process of the method, so that the method has great harm to human health and ecological environment; and the content of organic matters in the spinning solution exceeds 90%, and the surface of the fiber is not smooth and has more air holes after heat treatment.
Chinese patent literature, application publication number is: CN110670171A discloses a preparation method of a dense yttrium silicate ceramic fiber: yttrium nitrate, ethyl orthosilicate and TiSi 2 Adding the mixed solution into N-N dimethylformamide to obtain a mixed solution, carrying out wet ball milling on the mixed solution, adding polyvinylpyrrolidone into the mixed solution subjected to wet ball milling, stirring the mixed solution at room temperature, and standing the mixed solution after stirring to obtain a spinning solution; carrying out electrostatic spinning by using the spinning solution obtained in the step one to obtain composite fibers; carrying out heat treatment on the composite fiber obtained in the step two to obtain compact composite fiberYttrium silicate ceramic fibers. However, this patent introduces TiSi during the preparation process 2 This will greatly reduce the purity of the fiber, affecting product quality.
The traditional method for preparing ceramic fiber is to heat oxide raw material to a molten state, and to spin and form by a melting method. However, many specialty ceramic fibers have very high melting points and low melt viscosities, and are difficult to prepare by conventional methods. The sol-gel method solves this problem. The sol-gel method is a wet chemical method, and compared with the traditional method, the method has the advantages of good uniformity of chemical components, high product purity, easy control of the process, wide doping range, simple process equipment and the like, and is one of the commonly used methods for preparing glass fibers and polycrystalline ceramic fibers. The temperature of the sol-gel method is low, and when the sol reaches a proper viscosity, the sol can be spun and formed at room temperature, so that the method for preparing the yttrium silicate nano fiber with good spinnability by using the sol-gel method is an urgent need at present.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of yttrium silicate nanofiber and a preparation material thereof, which solve the problems in the prior art.
The preparation method of the yttrium silicate nanofiber comprises the following steps:
the method comprises the following steps: dripping a certain amount of catalytic liquid into tetraethoxysilane, and stirring to obtain silica sol; adding an yttrium source into the silica sol, and stirring to obtain yttrium silica sol; adding a spinning auxiliary agent into yttrium silica sol to obtain yttrium silicate precursor spinning solution;
step two: performing electrostatic spinning on the yttrium silicate precursor spinning solution obtained in the step one to obtain yttrium silicate precursor fibers;
step three: and (4) carrying out high-temperature heat treatment on the yttrium silicate precursor fiber obtained in the step two in an air environment to obtain an yttrium silicate nanofiber material product.
Further, in the first step, the catalytic solution is obtained by dissolving citric acid monohydrate in a solvent, wherein the solvent is a mixture of deionized water and ethanol or deionized water and methanol.
Further, in the step one, the component of the catalytic liquid, citric acid monohydrate: alcohol: the molar ratio of water is 0.01: (1-2): (6-7).
Further, in the first step, the yttrium source is one of or a combination of yttrium nitrate hexahydrate and yttrium chloride hexahydrate.
Further, in the step one, tetraethoxysilane: the molar ratio of the yttrium source is 1: (1-2).
Further, in the first step, the spinning aid is one of polyethylene oxide (PEO), polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), or a combination thereof.
Further, the mass ratio of the spinning auxiliary agent to the yttrium silicate precursor spinning solution is (0.015-0.12): 1;
furthermore, the viscosity of the yttrium silicate precursor spinning solution is 100-1000 mPas.
Further, the technological parameters of electrostatic spinning in the second step are as follows: the spinning voltage is 15-30 kV, the propelling speed is 0.6-1.5 mL/h, the receiving distance is 15-25 cm, the spinning humidity is 20-45%, and the spinning temperature is 20-40 ℃.
Further, during the high-temperature heat treatment in the third step, the temperature is raised to 1000-1500 ℃ at the temperature rise rate of 1-5 ℃/min, and the heat preservation time is 0.5-2 h.
The yttrium silicate nanofiber material disclosed by the invention is composed of yttrium silicate nano-crystalline grains, the diameter of the yttrium silicate nanofiber is 300-700nm, and no air holes or cracks exist on the surface of the fiber.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method and the preparation material of the yttrium silicate nanofiber, the yttrium silicate precursor spinning solution with good spinnability is prepared by a sol-gel method, and the yttrium silicate nanofiber with a compact structure is prepared by an electrostatic spinning technology. The fiber prepared by the method overcomes the defect that other components are introduced in the preparation process, improves the purity of the product and ensures the quality of the product.
The diameter of the prepared yttrium silicate nanofiber is 300-700nm, and the yttrium silicate nanofiber consists of yttrium silicate nano crystal grains; the fiber has compact structure on the micro scale, smooth surface, no air holes and cracks, high purity and wide application prospect in the fields of high-temperature heat insulation materials, structure reinforcing materials, flexible optical materials and the like. The method has the characteristics of simplicity, low cost, no pollution and good operability. The problems in the prior art are solved.
Drawings
FIG. 1 is an SEM photograph of yttrium silicate obtained by a preparation method of example 1;
fig. 2 is an XRD pattern of yttrium silicate of the preparation method of example 1.
Detailed Description
The invention is further illustrated by the following figures and examples:
example 1:
preferably, the preparation method of the yttrium silicate nanofiber comprises the following steps:
the method comprises the following steps: dissolving 2g of citric acid monohydrate in 18g of ethanol solution with the mass fraction of 18%, and fully stirring and dissolving to obtain a catalytic solution; dropwise adding 20g of catalytic liquid into 20.83g of ethyl orthosilicate, and stirring at a high speed for 6 hours to obtain uniform and transparent silica sol; adding 38.3g of yttrium nitrate into the silica sol, and fully stirring and dissolving to obtain yttrium silica sol; adding a spinning aid into yttrium silica sol, stirring for dissolving, stirring for 3-6 h, and adjusting the viscosity by using a solvent to prepare yttrium silicate precursor spinning solution; the spinning auxiliary agent is one or the combination of polyethylene oxide (PEO), polyvinylpyrrolidone (PVP) and polyvinyl alcohol (PVA); preferably, PVA is adopted, and is dissolved in an ethanol solution with the mass fraction of 30% to obtain a 12% PVA solution; adding PVA solution with equal mass into yttrium silica sol, and fully stirring for 3h to obtain yttrium silicate precursor spinning solution;
step two: and (3) performing electrostatic spinning on the yttrium silicate precursor spinning solution obtained in the step one at the temperature of 25 ℃ and the humidity of 40% to prepare yttrium silicate precursor fibers. The electrostatic spinning voltage is 30kV, the curing distance is 20cm, and the advancing speed is 0.8 mL/h.
Step three: heating the yttrium silicate precursor fiber obtained in the step two to 600 ℃ at the heating rate of 1 ℃/min in the air atmosphere, and preserving the heat for 2 h; then heating to 1300 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 2h to obtain the yttrium silicate nanofiber.
The working principle of the embodiment is as follows: an SEM photograph of the yttrium silicate fiber obtained by heat treatment at 1300 ℃ in the embodiment is shown in FIG. 1, and it can be seen from FIG. 1 that the yttrium silicate fiber with a compact structure prepared by the invention has a fiber diameter of 300-700nm, is composed of yttrium silicate nano-crystalline grains, and has no defects such as pores and cracks on the surface of the fiber.
The XRD pattern of the yttrium silicate fiber obtained by 1300 ℃ heat treatment of the embodiment is shown in figure 2. As can be seen from FIG. 2, the resulting fiber component is Y 2 Si 2 O 7 。
Example 2:
the yttrium silicate nanofiber prepared by the preparation method of the yttrium silicate nanofiber disclosed by the invention is composed of yttrium silicate nano crystal grains, the diameter of the yttrium silicate nanofiber is 300-700nm, and no air holes or cracks exist on the surface of the fiber. The material is used for high-temperature heat insulation materials, structural reinforcing materials, optical matrix materials, dielectric materials and the like.
The preparation method and the preparation material of the yttrium silicate nanofiber are described by combining the attached drawings, the yttrium silicate precursor spinning solution with good spinnability is prepared by a sol-gel method, and the yttrium silicate nanofiber with a compact structure is prepared by an electrostatic spinning technology. The fiber prepared by the method overcomes the defect that other components are introduced in the preparation process, improves the purity of the product and ensures the quality of the product. The problems in the prior art are solved. The present invention is not limited to the embodiments described, but rather, variations, modifications, substitutions and alterations of the embodiments may be made without departing from the spirit and scope of the present invention.

Claims (7)

1. A preparation method of yttrium silicate nano-fiber is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: dropping a certain amount of catalytic liquid into tetraethoxysilane, wherein the catalytic liquid is obtained by dissolving citric acid monohydrate in a solvent, the solvent is a mixture of deionized water and ethanol or the mixture of the deionized water and methanol, and the weight ratio of the citric acid monohydrate: alcohol: the molar ratio of water is 0.01: (1-2): (6-7), stirring to obtain silica sol; adding an yttrium source into the silica sol, and stirring to obtain yttrium silica sol; adding a spinning auxiliary agent into yttrium silica sol to obtain yttrium silicate precursor spinning solution; the viscosity of the yttrium silicate precursor spinning solution is 100-1000 mPa & s;
step two: performing electrostatic spinning on the yttrium silicate precursor spinning solution obtained in the step one to obtain yttrium silicate precursor fibers;
step three: carrying out high-temperature heat treatment on the yttrium silicate precursor fiber obtained in the step two in an air environment to obtain an yttrium silicate nanofiber material product; the yttrium silicate precursor spinning solution with good spinnability is prepared by adopting a sol-gel method, and the yttrium silicate nano-fiber with a compact structure is prepared by adopting an electrostatic spinning technology, wherein the yttrium silicate nano-fiber consists of yttrium silicate nano-crystalline grains, and the surface of the fiber has no air holes or crack defects.
2. The method of claim 1, wherein the yttrium silicate nanofibers are prepared by the steps of: in the first step, the yttrium source is one of or the combination of yttrium nitrate hexahydrate and yttrium chloride hexahydrate.
3. The method of claim 1, wherein the yttrium silicate nanofibers are prepared by the steps of: in the step one, tetraethoxysilane: the molar ratio of the yttrium source is 1: (1-2).
4. The method of claim 1, wherein the yttrium silicate nanofibers are prepared by the following steps: in the first step, the spinning auxiliary agent is one of or a combination of polyethylene oxide (PEO), polyvinylpyrrolidone (PVP) and polyvinyl alcohol (PVA).
5. The method of claim 1, wherein the yttrium silicate nanofibers are prepared by the following steps: the mass ratio of the spinning auxiliary agent to the yttrium silicate precursor spinning solution is (0.015-0.12): 1.
6. the method for preparing yttrium silicate nanofibers according to claim 1, wherein the process parameters of electrospinning in step two are as follows: spinning voltage is 15-30 kV, propelling speed is 0.6-1.5 mL/h, receiving distance is 15-25 cm, spinning humidity is 20-45%, and spinning temperature is 20-40 ℃; during the high-temperature heat treatment in the third step, the temperature is raised to 1000 ℃ and 1500 ℃ at the temperature raising rate of 1-5 ℃/min, and the heat preservation time is 0.5-2 h.
7. A yttrium silicate nanofiber material prepared according to the preparation method of any one of claims 1 to 6, characterized in that: the yttrium silicate nanofiber consists of yttrium silicate nano-crystalline grains, the diameter of the yttrium silicate nanofiber is 300-700nm, and no air holes or cracks exist on the surface of the fiber.
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CN1418992A (en) * 2001-11-14 2003-05-21 中国科学院山西煤炭化学研究所 Method for preparing silicon modified yttrium-aluminium garnet fibre
CN104003699B (en) * 2014-06-10 2016-08-17 中南大学 A kind of preparation method of yttrium silicate ceramic powders
CN104141181B (en) * 2014-07-22 2016-08-24 南京理工宇龙新材料科技有限公司 A kind of containing SiO2the ZrO of doping2the preparation method of fiber
CN104496469B (en) * 2014-12-18 2017-02-22 西安理工大学 Method for preparing dense micro/nano ceramic fiber by virtue of coaxial electrospinning technology
CN106927808B (en) * 2017-04-10 2020-05-01 山东大学 Preparation method of yttrium aluminum garnet continuous fibers
CN110670171B (en) * 2019-10-14 2022-03-29 齐齐哈尔大学 Preparation method of compact yttrium silicate ceramic fiber

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