CN110670171B - Preparation method of compact yttrium silicate ceramic fiber - Google Patents
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Abstract
A preparation method of compact yttrium silicate ceramic fiber, relating to a preparation method of ceramic fiber. Aims to solve the problem of low breaking strength of yttrium silicate fibers prepared by the existing electrostatic spinning method. 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; carrying out electrostatic spinning by using the spinning solution obtained in the step one to obtain composite fibers; and D, carrying out heat treatment on the composite fiber obtained in the step two to obtain the compact yttrium silicate ceramic fiber. 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. The invention is suitable for preparing the yttrium silicate ceramic fiber.
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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