CN111321475A - Inorganic fiber precursor spinning system and spinning method thereof - Google Patents
Inorganic fiber precursor spinning system and spinning method thereof Download PDFInfo
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- CN111321475A CN111321475A CN202010306104.0A CN202010306104A CN111321475A CN 111321475 A CN111321475 A CN 111321475A CN 202010306104 A CN202010306104 A CN 202010306104A CN 111321475 A CN111321475 A CN 111321475A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D7/00—Collecting the newly-spun products
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Abstract
The invention relates to an inorganic fiber precursor oriented spinning system and a spinning method thereof, wherein the spinning system comprises a precursor storage unit, a needle-shaped spinning unit, a control unit for controlling the needle-shaped spinning unit to directionally reciprocate and the injection speed, and a flat plate receiving unit, wherein the flat plate receiving unit is connected with the control unit and is used for receiving inorganic fiber precursors spun by the needle-shaped spinning unit. The spinning method is based on the spinning system and sets parameters of the control unit to spin. The spinning system can avoid the overlapping and crossing of the fiber protofilament in the spinning process, the application of the spinning system and the spinning method thereof can spin the inorganic fiber protofilament with controllable diameter and controllable length, and the chemical crosslinking and chemical reconstruction can be carried out under the condition of maintaining the appearance of the fiber protofilament in the processes of electron irradiation and curing crosslinking, thereby further ensuring that the stable and excellent inorganic high-performance fiber can be obtained in the sintering process.
Description
Technical Field
The invention relates to the technical field of fibers, in particular to an inorganic fiber precursor spinning system and a spinning method thereof.
Background
Inorganic high-performance fiber, such as silicon carbide fiber, silicon nitride fiber, alumina ceramic fiber, carbon fiber and the like, is one of typical representatives of high temperature resistance, high mechanical strength and corrosion resistance at present, and has unique application value in the fields of engineering material modification, engines, aerospace, ships, nuclear power equipment and the like. The main processes for preparing the inorganic fiber comprise the processes of precursor preparation, precursor spinning, fiber strand solidification, fiber strand sintering or carbonization and the like. The difficulty lies in spinning and fiber protofilament solidification, namely how to prepare the fiber protofilament with controllable diameter and controllable length, and chemical crosslinking and chemical reconstruction are carried out under the condition of maintaining the shape of the fiber protofilament so as to ensure that inorganic high-performance fiber with stability and excellent property is obtained in the sintering process.
Taking the silicon carbide fiber precursor polymer as an example, the curing of the silicon carbide polymer fiber precursor mainly comprises three methods, namely oxygen, chemical vapor and electron irradiation. Of these, electron irradiation is the most direct method of curing, however, the polymer precursor absorbs energy during irradiation to cause a temperature increase, which easily causes the fiber precursor to melt and lose the fiber structure. In addition, the fiber collecting method commonly used at present is a roller method, that is, the fiber polymer precursor is collected on a roller, and has the problems of non-uniform irradiation, concentrated heat, slow heat dissipation, high cost, and the like. The flat plate method or the net disk method is adopted, namely the fiber precursor is collected on a flat plate, so that the problems are easily overcome, but the key problem or difficulty of the flat plate collection method is how to prevent the fiber precursor from overlapping and crossing, thereby influencing the later electronic irradiation and influencing the uniformity of curing and crosslinking. And how to design a system or a method for arranging the inorganic fiber precursor on the net disc according to the orientation structure is expected to solve the problems, and meanwhile, the arrangement of the inorganic fiber precursor according to the orientation structure can improve the spinning efficiency and reduce the production cost.
Disclosure of Invention
The invention aims to design a fiber precursor spinning system and a fiber precursor spinning method, which can prepare inorganic fiber precursors with uniform sizes and distributed on a net disc according to an oriented structure.
In order to achieve the above purpose, the present application provides an inorganic fiber precursor orientation spinning system, which includes a precursor storage unit, a needle-shaped spinning unit, a control unit for controlling the movement track, the movement speed and the injection speed of the needle-shaped spinning unit, and a flat plate receiving unit matched with the needle-shaped spinning unit to form an inorganic fiber precursor arranged according to an orientation structure, wherein the flat plate receiving unit is connected with the control unit and used for receiving the inorganic fiber precursor spun by the needle-shaped spinning unit.
As a further improvement of the application, the flat plate receiving unit is a net disc with a temperature adjusting function.
As a further improvement of the present application, the mesh disc is circular or square.
As a further improvement of the application, the material of the net disc is any one of metal, ceramic and composite material.
As a further improvement of the present application, the control unit is a programmable controller.
In order to achieve the above object, the present application further provides an inorganic fiber precursor oriented spinning method, in which the inorganic fiber precursor oriented spinning system is applied, an inorganic fiber precursor is placed in the precursor storage unit, and the movement track, the movement speed, the injection speed of the needle-shaped spinning unit and the movement or rotation parameters of the flat plate receiving unit are set, so that the inorganic fiber precursors are arranged on the flat plate receiving unit according to the orientation structure.
As a further improvement of the application, the injection speed of the spinning needle of the needle-shaped spinning unit is more than 0 and less than V1 and less than or equal to 80L/h, and the moving speed of the spinning needle of the needle-shaped spinning unit is more than 0 and less than V2 and less than or equal to 20 m/s.
As a further improvement of the application, the temperature regulation range of the flat plate receiving unit is 10-200 ℃.
As a further improvement of the application, the rotation speed of the flat plate receiving unit is more than 0 and less than or equal to 4000 rpm.
As a further improvement of the present application, the precursor of the inorganic fiber precursor is at least one of polysilazane, polysilacarborane, polysilazane, and metal-containing polysilazane.
The beneficial effects of this application lie in, this application provides an inorganic fiber precursor orientation spinning system, store unit, needle-like spinning unit, control including the precursor needle-like spinning unit removes the control unit of orbit and translation rate and injection speed, with needle-like spinning unit cooperation forms the dull and stereotyped receiving element of inorganic fiber precursor according to the orientation structure of arranging, dull and stereotyped receiving element with the control unit links to each other and is used for receiving the inorganic fiber precursor that needle-like spinning unit spun. The inorganic fiber precursor orientation spinning system can avoid the overlapping and crossing of the fiber precursors in the spinning process, thereby influencing the later-stage electron irradiation and influencing the uniformity of curing and crosslinking. The application also provides an inorganic fiber precursor oriented spinning method, the inorganic fiber precursors with excellent performance and an oriented arrangement structure can be spun by the method, the diameter and the length are controllable, in the later electronic irradiation and curing crosslinking process, the chemical crosslinking and chemical reconstruction can be carried out under the maintenance of the morphology of the fiber precursors, and the stable inorganic high-performance fibers with excellent properties can be further obtained in the sintering process.
Drawings
FIG. 1 is a schematic structural diagram of an inorganic fiber precursor spinning system;
FIG. 2 is a schematic view of a single layer arrangement of inorganic fiber strands in a spiral orientation and extending outward from the center;
FIG. 3 is a schematic view of the inorganic fiber strands being oriented and arranged in an outward diverging manner with the mesh plate as the center;
FIG. 4 is a schematic view of the parallel arrangement of inorganic fiber strands in a wire mesh tray;
fig. 5 is a schematic view of a single layer arrangement of inorganic fiber strands oriented in a regular circular arrangement and extending outward from the center.
In the figure: 1. a precursor storage unit; 2. a needle-shaped spinning unit; 3. a flat panel receiving unit.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be described in detail and completely with reference to the following specific embodiments of the present application and the accompanying drawings. It should be apparent that the described embodiments are only some of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application. In the description of the present application, it is to be understood that the same or similar elements in different drawings are designated by the same reference numerals. The dimensions, proportions and number of elements are not intended to be limiting.
In order to realize the preparation of fiber precursors with controllable diameter and controllable length and maintain the shape of the fiber precursors to perform chemical crosslinking and chemical reconstruction so as to ensure that stable inorganic high-performance fibers with excellent properties are obtained in the sintering process, the application provides an inorganic fiber precursor oriented spinning system, as shown in fig. 1, the system comprises a precursor storage unit 1, a needle-shaped spinning unit 2, a control unit for controlling the moving track, the moving speed and the injection speed of the needle-shaped spinning unit 2, and a flat plate receiving unit 3 matched with the needle-shaped spinning unit 2 to form inorganic fiber precursors in oriented arrangement, wherein the flat plate receiving unit 3 is connected with the control unit and used for receiving the inorganic fiber precursors spun by the needle-shaped spinning unit 2. The needle-shaped spinning unit 2 comprises an electric control moving rod and a spinning needle head arranged on the electric control moving rod. Further, the loading capacity of the precursor storage unit 1 is more than 500L; the control unit indirectly controls the moving track and the moving speed of the spinning needle head and the injection speed of the spinning needle head by controlling the electric control moving rod.
In the present application, the flat panel receiving unit 3 is a mesh disc with a temperature adjusting function, as a further improvement of the present application, the mesh disc is circular or square, and the size range of the mesh disc is not limited; the net disc is made of any one of metal, ceramic and composite materials; the temperature regulation range of the net disc is 10-200 ℃, and the preferable temperature is 30-150 ℃; the control unit is a programmable controller.
In the application, an inorganic fiber precursor orientation spinning method is also provided, and by applying the inorganic fiber precursor orientation spinning device, an inorganic fiber precursor is placed in the precursor storage unit 1, the moving track, the moving speed and the injection speed of the spinning needle of the needle-shaped spinning unit 2 are adjusted, the moving or rotating parameters of the flat plate receiving unit 3 are set, and the inorganic fiber precursors are arranged on the flat plate receiving unit 3 according to the orientation structure.
In the present application, the injection speed of the spinning needle of the needle-shaped spinning unit 2 is 0 < V1 < 80L/h, V1 represents the injection speed of the spinning needle of the needle-shaped spinning unit 2, and more preferably, the injection speed of the spinning needle of the needle-shaped spinning unit 2 is 0 < V1 < 50L/h; the needle moving speed of the needle-shaped spinning unit 2 is more than 0 and less than or equal to V2 and less than or equal to 20m/s, V2 represents the moving speed of the spinning needle, and further preferably, the moving speed of the spinning needle of the needle-shaped spinning unit 2 is more than or equal to 0.2m/s and less than or equal to V2 and less than or equal to 10 m/s; the rotating speed of the flat plate receiving unit 3 is 0 < r ≦ 4000rpm, r represents the rotating speed of the flat plate receiving unit 3, and more preferably 100rpm < r ≦ 3500 rpm. The precursor of the inorganic fiber precursor is an organic solvent or sol, wherein the organic solvent is any one or the combination of more than two of polysilazane, polysilacarborane, polysilazane and metal-containing polysilazane; the solution for preparing the sol is any one or the combination of more than two of ethanol, methanol, tetrahydrofuran, N-methyl pyrrolidone, N-dimethylformamide, dimethyl sulfoxide, benzene, toluene, N-hexane and N-heptane, and the mass content of the precursor in the precursor sol of the inorganic fiber precursor is 30-70%.
In order to verify the excellent performance of the inorganic fiber strand oriented spinning system, some examples are also provided herein for reference.
Example 1
Firstly, 500L of polysilazane sol is put into a precursor storage unit 1; secondly, preheating a circular net disc made of SiC material to 150 ℃, and rotating at the speed of 100 rpm; setting parameters of a control unit, setting the injection speed of the needle-shaped spinning unit 2 to be 10L/h, and setting the moving speed of an electric control moving rod to enable the moving speed of a spinning needle head arranged on the electric control moving rod to be 0.2 m/s; and finally, starting the needle-shaped spinning unit 2, spinning the polysilazane sol onto a flat plate receiving unit 3, wherein the flat plate receiving unit 3 is a circular mesh plate made of SiC, and the polysilazane sol protofilament forms a silicon carbide fiber protofilament which is spirally oriented and is arranged in a single layer and extends outwards from the center on the mesh plate, the diameter of the fiber protofilament is 80 micrometers, and the length of the fiber protofilament is 1 ten kilometer.
Example 2
Firstly, 600L of polysilazane sol is put into a precursor storage unit 1; secondly, preheating a circular mesh plate made of zirconia to 150 ℃, and rotating at 3500 rpm; setting parameters of a control unit, setting the injection speed of the needle-shaped spinning unit 2 to be 50L/h, and setting the moving speed of an electric control moving rod to enable the moving speed of a spinning needle head arranged on the electric control moving rod to be 10 m/s; and finally, starting the needle-shaped spinning unit 2, spinning the polysilazane sol onto a flat plate receiving unit 3, wherein the flat plate receiving unit 3 is a circular mesh plate made of zirconia, and the polysilazane sol protofilament forms a silicon carbide fiber protofilament which is spirally oriented and is arranged in a single layer and extends outwards from the center on the mesh plate, the diameter of the fiber protofilament is 20 micrometers, and the length of the fiber protofilament is 1.5 kilometers.
Example 3
Firstly, 700L of polysilazane sol is put into a precursor storage unit 1; secondly, preheating a circular net disc made of SiC material to 35 ℃, and rotating at the speed of 1500 rpm; setting parameters of a control unit, setting the injection speed of the needle-shaped spinning unit 2 to be 8L/h, and setting the moving speed of an electric control moving rod to enable the moving speed of a spinning needle head arranged on the electric control moving rod to be 8 m/s; and finally, starting the needle-shaped spinning unit 2, spinning the polysilazane sol onto a flat plate receiving unit 3, wherein the flat plate receiving unit 3 is a circular mesh plate made of SiC, and the polysilazane sol protofilament forms a silicon carbide fiber protofilament which is spirally oriented and is arranged in a single layer and extends outwards from the center on the mesh plate, the diameter of the fiber protofilament is 30 micrometers, and the length of the fiber protofilament is 2.5 kilometers.
Example 4
Firstly, 650L of polysilazane-carbonitride sol is put into a precursor storage unit 1; secondly, preheating a circular net disk made of metal tungsten to 100 ℃, and rotating in a discontinuous mode; setting parameters of a control unit, setting the injection speed of the needle-shaped spinning unit 2 to be 15L/h, and setting the moving speed of an electric control moving rod to enable the moving speed of a spinning needle head arranged on the electric control moving rod to be 20 m/s; finally, the needle-shaped spinning unit 2 is started to spin the poly-silicon-carbon-nitrogen sol on the flat plate receiving unit 3, as shown in fig. 3, the flat plate receiving unit 3 is a circular mesh plate made of metal tungsten, the poly-silicon-carbon-nitrogen sol protofilament forms silicon-carbon-nitrogen fiber protofilaments which are diffused outwards on the mesh plate, the silicon-carbon-nitrogen fiber protofilament is in a divergent orientation arrangement, the diameter of the silicon-carbon-nitrogen fiber protofilament is 15 micrometers, and the length of each fiber is the same as the radius of the circular plate.
Example 5
Firstly, 600L of poly-silicon carbon nitrogen alkane sol is put into a precursor storage unit 1; secondly, preheating a square mesh plate made of metal tungsten to 100 ℃; setting parameters of a control unit, setting the injection speed of the needle-shaped spinning unit 2 to be 45L/h, and setting the moving speed of an electric control moving rod, so that the moving speed of a spinning needle head arranged on the electric control moving rod is 10m/s, and the needle head is translated by 29 micrometers when moving to the edge of a mesh disc; finally, the needle-shaped spinning unit 2 is started to spin the polysilazane/carbonitride sol onto the flat plate receiving unit 3, as shown in fig. 4, the flat plate receiving unit 3 is a square mesh plate made of metal tungsten, the polysilazane/carbonitride sol precursor forms silicon/carbon/nitrogen fiber precursor fibers arranged in parallel on the mesh plate, the diameter of the fiber precursor is 15 μm, and the length of each fiber is equal to the length of the long side of the square mesh plate.
Example 6
Firstly, 550L of poly-silicon carborane sol is put into a precursor storage unit 1; secondly, preheating a circular mesh plate made of zirconia to 100 ℃, and rotating at the speed of 1000 rpm; setting parameters of a control unit, setting the injection speed of the needle-shaped spinning unit 2 to be 5L/h, and setting the moving speed of an electric control moving rod to enable the moving speed of a spinning needle head arranged on the electric control moving rod to be 2 m/s; and finally, starting the needle-shaped spinning unit 2, spinning the polycarborane sol onto a flat plate receiving unit 3, wherein the flat plate receiving unit 3 is a circular mesh plate made of zirconium oxide, and the polycarborane sol protofilament forms a single-layer silicon arborane fiber protofilament which is arranged in a regular circular arrangement and oriented and is expanded from the center to the outside on the mesh plate, the diameter of the fiber protofilament is 10 micrometers, and the length of each circle of the fiber is from 1 meter to 150 meters.
To sum up, the application provides an inorganic fiber precursor orientation spinning system, including precursor storage unit 1, needle-like spinning unit 2, control needle-like spinning unit 2 removes the control unit of orbit and translation rate and injection speed, with needle-like spinning unit 2 cooperates and forms inorganic fiber precursor and follows the dull and stereotyped receiving element 3 that the orientation structure was arranged, dull and stereotyped receiving element 3 with control unit links to each other and is used for receiving the inorganic fiber precursor that needle-like spinning unit 2 spun out. The inorganic fiber precursor oriented spinning system can avoid the overlapping and crossing of the fiber precursors in the spinning process, thereby influencing the later-stage electron irradiation and influencing the uniformity of curing and crosslinking.
The application also provides an inorganic fiber precursor orientation spinning method, which is characterized in that the inorganic fiber precursor orientation spinning system is applied, an inorganic fiber precursor is placed in the precursor storage unit 1, the moving track, the moving speed and the injection speed of the needle-shaped spinning unit 2 are adjusted, the moving or rotating parameters of the flat plate receiving unit 3 are set, and the inorganic fiber precursors are arranged on the flat plate receiving unit 3 according to the orientation structure. The method can be used for spinning the inorganic fiber precursor uniformly distributed according to the orientation structure, the concentration of the inorganic fiber precursor is controlled in a proper range, the moving track, the moving speed and the injection speed of the spinning needle head are adjusted, the material, the temperature and the moving or rotating parameters of the flat plate receiving unit 3 are adjusted, the diameter and the length of the inorganic fiber precursor are controllable, further, in the later electronic irradiation and curing crosslinking processes, the chemical crosslinking and the chemical reconstruction can be carried out under the condition that the morphology of the fiber precursor is maintained, and the stable inorganic high-performance fiber with excellent properties can be further obtained in the sintering process.
The present application has been described in connection with only the presently preferred embodiments with the understanding that the present disclosure is not to be considered as limiting, and the present application is not limited to the examples described above, but rather, it is to be understood that changes, modifications, additions or substitutions that are within the spirit and scope of the application by one of ordinary skill in the art are included.
Claims (10)
1. The inorganic fiber precursor orientation spinning system is characterized by comprising a precursor storage unit (1), needle-shaped spinning units (2), a control unit for controlling the moving tracks, the moving speed and the injection speed of the needle-shaped spinning units (2), and a flat plate receiving unit (3) matched with the needle-shaped spinning units (2) to form inorganic fiber precursors arranged according to an orientation structure, wherein the flat plate receiving unit (3) is connected with the control unit and is used for receiving the inorganic fiber precursors spun by the needle-shaped spinning units (2).
2. The inorganic fiber strand orientation spinning system according to claim 1, wherein the flat plate receiving unit (3) is a screen pan having a temperature-adjustable function.
3. An inorganic fiber strand orientation spinning system as in claim 2, wherein the screen disks are circular or square.
4. The inorganic fiber strand oriented spinning system of claim 2, wherein the material of the mesh disk is any one of metal, ceramic and composite material.
5. An inorganic fiber strand orientation spinning system as claimed in claim 1, wherein said control unit is a programmable controller.
6. An inorganic fiber precursor oriented spinning method is characterized in that the inorganic fiber precursor oriented spinning system of any one of claims 1 to 5 is applied, an inorganic fiber precursor is placed in the precursor storage unit (1), and the movement track, the movement speed and the injection speed of the needle-shaped spinning unit (2) and the movement or rotation parameters of the flat plate receiving unit (3) are set, so that the inorganic fiber precursor is arranged on the flat plate receiving unit (3) according to an oriented structure.
7. The method for oriented spinning of inorganic fiber strands according to claim 6, wherein the injection speed of the needle-like spinning unit (2) is 0 < V1 < 80L/h, and the moving speed of the needle-like spinning unit (2) is 0 < V2 < 20 m/s.
8. The inorganic fiber strand orientation spinning method according to claim 6, wherein the temperature control range of the flat plate receiving unit (3) is 10 ℃ to 200 ℃.
9. The method for oriented spinning of inorganic fiber strands according to claim 6, wherein the rotation speed of the plate-receiving unit (3) is 0 < r.ltoreq.4000 rpm.
10. The method for oriented spinning of inorganic fiber strands according to claim 6, wherein the precursor of the inorganic fiber strands is at least one of polysilazane, polysilacarborane, polysilazane, and metal-containing polysilazane.
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| PB01 | Publication | ||
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Application publication date: 20200623 |