CN110670171B - Preparation method of compact yttrium silicate ceramic fiber - Google Patents
Preparation method of compact yttrium silicate ceramic fiber Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 99
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 44
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000000919 ceramic Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000000243 solution Substances 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000009987 spinning Methods 0.000 claims abstract description 23
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 18
- 239000011148 porous material Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910008484 TiSi Inorganic materials 0.000 claims abstract description 12
- 238000010041 electrostatic spinning Methods 0.000 claims description 22
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910008479 TiSi2 Inorganic materials 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- 238000003746 solid phase reaction Methods 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 238000001523 electrospinning Methods 0.000 abstract 2
- 239000004698 Polyethylene Substances 0.000 abstract 1
- NVZBIFPUMFLZLM-UHFFFAOYSA-N [Si].[Y] Chemical compound [Si].[Y] NVZBIFPUMFLZLM-UHFFFAOYSA-N 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- -1 polyethylene Polymers 0.000 abstract 1
- 229920000573 polyethylene Polymers 0.000 abstract 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 4
- 239000002121 nanofiber Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000006250 one-dimensional material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
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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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63444—Nitrogen-containing polymers, e.g. polyacrylamides, polyacrylonitriles, polyvinylpyrrolidone [PVP], polyethylenimine [PEI]
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- 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
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Abstract
一种致密硅酸钇陶瓷纤维的制备方法，涉及一种陶瓷纤维的制备方法。目的是解决现有静电纺丝方法制备的硅酸钇纤维的断裂强度低的问题。方法：将硝酸钇、正硅酸乙酯和TiSi2加入到N‑N二甲基甲酰胺中，得到混合液，对混合液进行湿法球磨，向湿法球磨后的混合液中添加聚乙烯吡咯烷酮并在室温下搅拌混合液，搅拌完成后静置，得到纺丝液；利用步骤一得到的纺丝液进行静电纺丝，得到复合纤维；将步骤二得到的复合纤维进行热处理，得到致密硅酸钇陶瓷纤维。本发明制备得到的Y2Si2O5纤维表面光滑且无孔隙，硅酸钇纤维的断裂强度显著提高，达到6MPa。本发明适用于制备硅酸钇陶瓷纤维。
A preparation method of dense yttrium silicate ceramic fiber relates to a preparation method of ceramic fiber. The purpose is to solve the problem of low breaking strength of the yttrium silicate fiber prepared by the existing electrospinning method. Method: add yttrium nitrate, ethyl orthosilicate and TiSi into N - N dimethylformamide to obtain a mixed solution, carry out wet ball milling to the mixed solution, and add polyethylene to the mixed solution after wet ball milling pyrrolidone and the mixed solution is stirred at room temperature, and after the stirring is completed, it is left to stand to obtain a spinning solution; the spinning solution obtained in step 1 is used for electrospinning to obtain composite fibers; the composite fibers obtained in step 2 are subjected to heat treatment to obtain dense silicon Yttrium acid ceramic fiber. The Y 2 Si 2 O 5 fiber prepared by the invention has a smooth surface and no pores, and the breaking strength of the yttrium silicate fiber is significantly improved, reaching 6MPa. The invention is suitable for preparing yttrium silicate ceramic fibers.
Description
Technical Field
The invention relates to a preparation method of ceramic fiber.
Background
The ceramic fiber is a fibrous light refractory material, and has the advantages of light weight, high temperature resistance, good thermal stability, low thermal conductivity, small specific heat, mechanical shock resistance and the like. In the composite material prepared by compounding the ceramic fiber and the ceramic, the ceramic fiber is taken as the toughening fiber, thus breaking the single problemThe brittleness of the ceramic and the toughness of the composite material are improved. One common ceramic fiber is yttrium silicate fiber, which includes Y2Si2O5、Y2Si2O7And Y4Si3O12Three crystal phase structures, wherein Y2Si2O5And Y2Si2O7Melting points of (A) are 1980 ℃ and 1775 ℃ respectively, and are most common; the yttrium silicate has the characteristics of high melting point, low thermal expansion coefficient, low evaporation rate, low oxygen permeability, low modulus, low thermal conductivity, good chemical stability and thermal stability and the like.
In recent years, the technology for preparing inorganic nanofibers by utilizing the electrostatic spinning technology is more and more concerned, the inorganic nanofibers prepared by the method break through the particle form of the traditional inorganic material, the specific surface area of the fibers is large, the length-diameter ratio is large, the surface energy and the activity are high, and the inorganic nanofibers can be applied to a plurality of high-value fields. The prior literature discloses that the yttrium silicate fiber can be prepared by utilizing an electrostatic spinning technology, but the method causes a large amount of pores on the surface of the fiber due to the decomposition of organic matters in the spinning process, so that the prepared yttrium silicate fiber has a porous structure on the surface, and the breaking strength of the fiber is low and is only 4.5MPa at most.
Disclosure of Invention
The invention provides a preparation method of compact yttrium silicate ceramic fiber, aiming at solving the problem of low breaking strength of yttrium silicate fiber prepared by the existing electrostatic spinning method.
The preparation method of the compact yttrium silicate ceramic fiber is carried out according to the following steps:
the method comprises the following steps: yttrium nitrate, ethyl orthosilicate and TiSi2Adding 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;
step two: carrying out electrostatic spinning by using the spinning solution obtained in the step one to obtain composite fibers;
step three: and D, carrying out heat treatment on the composite fiber obtained in the step two to obtain the compact yttrium silicate ceramic fiber.
The principle and the beneficial effects of the invention are as follows:
the invention uses yttrium nitrate as a Y source, ethyl orthosilicate as a Si source, polymer solution containing the Y source and the Si source is subjected to electrostatic spinning to obtain composite fiber, organic matters are removed from the composite fiber in the heat treatment process and subjected to solid-phase reaction to finally obtain yttrium silicate fiber, but the organic matters are decomposed during removal to cause a large amount of pores on the surface of the fiber2Oxidation to SiO at high temperature2And TiO2And SiO2And TiO2The mixture of (A) grows in the pores on the already formed yttrium silicate fibers and gradually accumulates to finally fill the pores, while SiO2、TiO2And the yttrium silicate generates solid phase reaction during heat treatment to realize mutual bonding, and finally the formed yttrium silicate fiber is a compact polycrystalline sintered body, and pores in the fiber disappear.
Y prepared by the invention2Si2O5The surface of the fiber is smooth and has no pores, and the breaking strength of the yttrium silicate fiber is obviously improved to 6 MPa.
Drawings
FIG. 1 is Y prepared in example 12Si2O5XRD spectrum of the fiber;
FIG. 2 is Y prepared in example 12Si2O5SEM photograph of fiber morphology;
FIG. 3 shows Y obtained in example 22Si2O5SEM photograph of fiber morphology;
FIG. 4 shows Y obtained in example 32Si2O5SEM photograph of fiber morphology;
FIG. 5 shows Y obtained in example 42Si2O5SEM photograph of fiber morphology.
The specific implementation mode is as follows:
the technical scheme of the invention is not limited to the specific embodiments listed below, and any reasonable combination of the specific embodiments is included.
The first embodiment is as follows: the preparation method of the dense yttrium silicate ceramic fiber of the embodiment is carried out according to the following steps:
the method comprises the following steps: yttrium nitrate, ethyl orthosilicate and TiSi2Adding 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; the polyvinylpyrrolidone is used for adjusting the viscosity of the spinning solution;
step two: carrying out electrostatic spinning by using the spinning solution obtained in the step one to obtain composite fibers;
step three: and D, carrying out heat treatment on the composite fiber obtained in the step two to obtain the compact yttrium silicate ceramic fiber.
In the embodiment, yttrium nitrate is used as a Y source, ethyl orthosilicate is used as a Si source, a polymer solution containing the Y source and the Si source is subjected to electrostatic spinning to obtain composite fibers, organic matters are removed from the composite fibers in the heat treatment process and subjected to solid-phase reaction to finally obtain yttrium silicate fibers, but the organic matters are decomposed during removal to cause a large amount of pores on the surfaces of the fibers2Oxidation to SiO at high temperature2And TiO2And SiO2And TiO2The mixture of (A) grows in the pores on the already formed yttrium silicate fibers and gradually accumulates to finally fill the pores, while SiO2、TiO2And the yttrium silicate generates solid phase reaction during heat treatment to realize mutual bonding, and finally the formed yttrium silicate fiber is a compact polycrystalline sintered body, and pores in the fiber disappear. Y produced in the present embodiment2Si2O5The surface of the fiber is smooth and has no pores, and the breaking strength of the yttrium silicate fiber is obviously improved to 6 MPa.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: step one, adding polyvinylpyrrolidone into the mixed solution after wet ball milling, stirring the mixed solution at room temperature for 5.5-6.5 h, and standing for 1.5-2.5 h after stirring. Other steps and parameters are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: step one, the wet ball milling time is 11.5-12.5 h; the grinding balls adopted in the ball milling process are alumina balls, and the ball-to-material ratio is 1: (3-5), the rotating speed of the ball mill is 240-260 r/min. Other steps and parameters are the same as in the first embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: step one, TiSi in the mixed liquid2The mass fraction of (A) is 14.5-15.5%. Other steps and parameters are the same as in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: step one, TiSi in the mixed liquid2And yttrium nitrate in a molar ratio of 1: (2-3). Other steps and parameters are the same as in one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: step one, the molar ratio of yttrium nitrate to tetraethoxysilane in the mixed solution is 1 (1-2). Other steps and parameters are the same as in one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: step one, the molar ratio of yttrium nitrate to polyvinylpyrrolidone in the spinning solution is 1: (1-2). Other steps and parameters are the same as in one of the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: injecting the spinning solution into a solution storage pipe of an electrostatic spinning machine before the electrostatic spinning process is carried out, wherein the electrostatic spinning process comprises the following steps: the inner diameter of the adopted spray head is 0.45-0.55 mm, the curing distance is 19-21 cm, the included angle between the spray head and the horizontal plane is 19-21 degrees, the applied direct current voltage is 19.5-20.5 kV, the environmental temperature is 20-25 ℃, and the humidity of the air is 40-50%. Other steps and parameters are the same as in one of the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and step three, during heat treatment, the atmosphere is inert gas protective atmosphere, during heat treatment, the temperature is raised to 1350-1450 ℃ at the temperature rise rate of 4.9-5.1 ℃/min, the temperature is kept for 2.8-3.2 hours, then the temperature is lowered to 190-210 ℃ at the temperature drop rate of 4.9-5.1 ℃/min, and finally the temperature is lowered to the room temperature along with the furnace. Other steps and parameters are the same as in one of the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: and step three, the device adopted by the heat treatment is a program temperature control furnace, such as a vacuum tube type atmosphere furnace. Other steps and parameters are the same as in one of the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1:
the preparation method of the dense yttrium silicate ceramic fiber of the embodiment is carried out according to the following steps:
the method comprises the following steps: yttrium nitrate, ethyl orthosilicate and TiSi2Adding 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 for 6 hours, and standing for 2 hours after stirring is finished to obtain a spinning solution;
the wet ball milling time is 12 hours; the grinding balls adopted in the ball milling process are alumina balls, and the ball-to-material ratio is 1: 4, the rotating speed of the ball mill is 250 r/min;
TiSi in the mixed solution2The mass fraction of (A) is 15%;
TiSi in the mixed solution2And yttrium nitrate in a molar ratio of 1: 3;
the molar ratio of yttrium nitrate to tetraethoxysilane in the mixed solution is 1: 1;
the molar ratio of yttrium nitrate to polyvinylpyrrolidone in the spinning solution is 1: 1;
step two: carrying out electrostatic spinning by using the spinning solution obtained in the step one to obtain composite fibers;
before the electrostatic spinning process, the spinning solution is injected into a solution storage pipe of an electrostatic spinning machine, and in the electrostatic spinning process: the inner diameter of a spray head is 0.5mm, the curing distance is 20cm, the included angle between the spray head and the horizontal plane is 20 degrees, the applied direct-current voltage is 20kV, the ambient temperature is 22 ℃, and the humidity of air is 45 percent;
step three: carrying out heat treatment on the composite fiber obtained in the step two to obtain compact yttrium silicate ceramic fiber;
the atmosphere during the heat treatment is inert gas protective atmosphere, the temperature is increased to 1400 ℃ at the temperature increasing rate of 5 ℃/min and is kept for 3 hours during the heat treatment, then the temperature is reduced to 200 ℃ at the temperature decreasing rate of 5 ℃/min, and finally the temperature is reduced to room temperature along with the furnace; the device adopted by the heat treatment is a vacuum tube type atmosphere furnace.
FIG. 1 is Y prepared in example 12Si2O5XRD spectrum of the fiber; FIG. 1 shows Y prepared2Si2O5The ceramic fiber has good crystallinity and is similar to standard card Y2SiO5(PDF 52-1810) are identical.
FIG. 2 is Y prepared in example 12Si2O5SEM photograph of fiber morphology; as can be seen in FIG. 2, Y2Si2O5The degree of densification of the fiber surface is high, so when TiSi is used2The repair effect is most excellent when the doping amount of (A) is 15%.
Example 2:
the preparation method of the dense yttrium silicate ceramic fiber of the embodiment is carried out according to the following steps:
the method comprises the following steps: adding yttrium nitrate and tetraethoxysilane into N, N-dimethylformamide to obtain a mixed solution, adding polyvinylpyrrolidone into the mixed solution, stirring at room temperature for 6 hours, and standing for 2 hours after stirring is completed to obtain a spinning solution;
the mass fraction of yttrium nitrate in the spinning solution is 22%;
the molar ratio of yttrium nitrate to tetraethoxysilane in the mixed solution is 1: 1;
the molar ratio of yttrium nitrate to polyvinylpyrrolidone in the spinning solution is 1: 1;
step two: carrying out electrostatic spinning by using the spinning solution obtained in the step one to obtain composite fibers;
before the electrostatic spinning process, the spinning solution is injected into a solution storage pipe of an electrostatic spinning machine, and in the electrostatic spinning process: the inner diameter of a spray head is 0.5mm, the curing distance is 20cm, the included angle between the spray head and the horizontal plane is 20 degrees, the applied direct-current voltage is 20kV, the ambient temperature is 22 ℃, and the humidity of air is 45 percent;
step three: carrying out heat treatment on the composite fiber obtained in the step two to obtain compact yttrium silicate ceramic fiber;
the atmosphere during the heat treatment is air atmosphere, the temperature is increased to 1400 ℃ at the temperature increasing rate of 5 ℃/min and is kept for 3 hours during the heat treatment, then the temperature is reduced to 200 ℃ at the temperature decreasing rate of 5 ℃/min, and finally the temperature is reduced to room temperature along with the furnace; the device adopted by the heat treatment is a vacuum tube type atmosphere furnace.
FIG. 3 shows Y obtained in example 22Si2O5SEM photograph of fiber morphology; example 2 undoped TiSi2FIG. 3 shows Y obtained in example 22Si2O5The ceramic fibers were porous fibers and tested, Y from example 22Si2O5The breaking strength of the fiber was 4.4 MPa.
Example 3:
this example differs from example 1 in that: step one, TiSi in the mixed solution2Was 10% by mass, and the other steps and parameters were the same as in example 1.
FIG. 4 shows Y obtained in example 32Si2O5SEM photograph of fiber morphology; as can be seen in FIG. 4, Y2Si2O5Incomplete repair of fibers, Y2Si2O5There are still more voids in the fibers. Y obtained in example 32Si2O5The breaking strength of the fiber was 4.6 MPa.
Example 4:
this example differs from example 1 in that: step one, TiSi in the mixed solution2Was 20% by mass, and the other steps and parameters were the same as in example 1.
FIG. 5 shows Y obtained in example 42Si2O5Morphology of the fibersSEM photograph of (a); as can be seen in FIG. 5, Y2Si2O5The surface of the fiber is raised, and the smoothness of the surface of the fiber is influenced by the presence of the protrusions, namely, the performance of the one-dimensional material of the fiber is damaged, and the toughening effect of the fiber is reduced. Y obtained in example 42Si2O5The breaking strength of the fiber was 4.8 MPa.
As can be seen from FIGS. 2 to 5, Y in example 12Si2O5TiSi of fibers2The doping amount of the silicon dioxide is 15 percent, the repairing effect is most excellent when the heat treatment temperature is 1400 ℃, and the prepared Y2Si2O5The diameter of the fiber is 300nm, Y2Si2O5The fiber surface is smooth and has no pores, the fracture strength of the yttrium silicate fiber is obviously improved, and the TiSi is tested2The doping amount of the yttrium silicate fiber is 15 percent, and the breaking strength of the prepared yttrium silicate fiber reaches 6MPa when the heat treatment temperature is 1400 ℃.
Claims (6)
1. A preparation method of compact yttrium silicate ceramic fiber is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: yttrium nitrate, ethyl orthosilicate and TiSi2Adding 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;
TiSi in the mixed solution2The mass fraction of (A) is 14.5-15.5%;
TiSi in the mixed solution2And yttrium nitrate in a molar ratio of 1: (2-3);
the molar ratio of yttrium nitrate to tetraethoxysilane in the mixed solution is 1 (1-2);
step two: carrying out electrostatic spinning by using the spinning solution obtained in the step one to obtain composite fibers;
step three: carrying out heat treatment on the composite fiber obtained in the step two to obtain compact yttrium silicate ceramic fiber;
TiSi2oxygen at high temperatureIs converted into SiO2And TiO2The mixture of (2) grows in the pores on the already formed yttrium silicate fibers, filling the pores with SiO simultaneously2、TiO2The yttrium silicate and yttrium silicate generate solid phase reaction during heat treatment to realize mutual bonding, and finally the formed yttrium silicate fiber is a compact polycrystalline sintered body, and pores in the fiber disappear;
and during heat treatment, the atmosphere is inert gas protective atmosphere, the temperature is raised to 1350-1450 ℃ at the temperature rise rate of 4.9-5.1 ℃/min and is kept for 2.8-3.2 h, then the temperature is lowered to 190-210 ℃ at the temperature reduction rate of 4.9-5.1 ℃/min, and finally the temperature is lowered to room temperature along with the furnace.
2. The method of preparing densified yttrium silicate ceramic fiber of claim 1, wherein: step one, adding polyvinylpyrrolidone into the mixed solution after wet ball milling, stirring the mixed solution at room temperature for 5.5-6.5 h, and standing for 1.5-2.5 h after stirring.
3. The method of preparing densified yttrium silicate ceramic fiber of claim 1, wherein: step one, the wet ball milling time is 11.5-12.5 h; the grinding balls adopted in the ball milling process are alumina balls, and the ball-to-material ratio is 1: (3-5), the rotating speed of the ball mill is 240-260 r/min.
4. The method of preparing densified yttrium silicate ceramic fiber of claim 1, wherein: step one, the molar ratio of yttrium nitrate to polyvinylpyrrolidone in the spinning solution is 1: (1-2).
5. The method of preparing densified yttrium silicate ceramic fiber of claim 1, wherein: injecting the spinning solution into a solution storage pipe of an electrostatic spinning machine before the electrostatic spinning process is carried out, wherein the electrostatic spinning process comprises the following steps: the inner diameter of a spray head is 0.45-0.55 mm, the curing distance is 19-21 cm, the included angle between the spray head and the horizontal plane is 19-21 degrees, the applied direct-current voltage is 19.5-20.5 kV, the ambient temperature is 20-25 ℃, and the humidity of air is 40-50%.
6. The method of preparing densified yttrium silicate ceramic fiber of claim 1, wherein: and step three, the device adopted by the heat treatment is a program temperature control furnace.
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