KR20210037497A - Continuous infusible treatment device on pcs fiber - Google Patents

Abstract

A device for continuous infusibility of PCS fibers comprises a guide tube and a heating unit. The guide tube is connected to one side of a melt spinning unit, and a curing gas is injected and discharged therein. The heating unit includes a heating element surrounding the guide tube and a reflector surrounding the heating element, and applies heat to the PCS fibers in the guide tube. Through the device for continuous infusibility of PCS fibers, the melt spinning and curing (infusibility) processes proceed continuously.

Description

Continuous infusion device of PCS fiber TECHNICAL FIELD {CONTINUOUS INFUSIBLE TREATMENT DEVICE ON PCS FIBER}

The present invention relates to a device for continuous infusible of PCS fibers and a method for continuous infusible thereof. More specifically, it relates to a device for continuously performing a melt spinning process and an infusible process of PCS fibers, and a continuous infusible method thereof.

Silicon carbide (SiC) fiber is a fiber manufactured at high temperatures under an inert atmosphere.Since it has excellent mechanical properties at ultra-high temperatures, recently space aircraft engines, nuclear power plant internal structures, thermal power plant turbine blades, brake pads/discs, and built-in guided weapons It is widely used in various fields such as parts and semiconductor fixtures.

The raw material for producing SiC fibers is polycarbosilane (PCS). In general, the manufacturing method of SiC fiber includes a step of melt spinning PCS as a raw material to form a fibrous form, a chemical treatment step of converting the PCS fiber from thermoplastic to thermosetting (incompatibility step), and PCS fiber converted to heat curable. It consists of a heat treatment step of heat treatment at least about 1000 ℃ or more in an inert atmosphere to convert the ceramic.

In order to manufacture SiC fibers through such a method, it is necessary to undergo a curing process (infusible treatment process) for converting thermoplastic PCS fibers supplied through melt spinning of polymer PCS as a starting material into thermosetting properties. However, as described in Korean Patent Publication No. 10-1848383, PCS fibers supplied through melt spinning are very weak, and during chemical treatment of several strands of PCS fibers into bundles, heat for each location such as the surface, center, and bottom There is a difference in the degree of conversion to hardenability, and damage due to handling occurs during winding and rewinding of the PCS fiber in the chemical treatment step, thereby significantly reducing the quality (e.g., strength) of the finally produced SiC fiber. There is a problem.

In addition, according to the conventional SiC fiber manufacturing method, the PCS fiber produced through melt spinning is wound around a bobbin of a winder. To perform the chemical treatment step, the bobbin is separated from the winder and PCS fiber bundles should be unwound from In this way, there is a risk that the PCS fiber is disconnected or damaged in the process of winding and rewinding the PCS fiber on the bobbin. SiC fibers that are finally manufactured by heat-treating the disconnected or broken PCS fibers may have poor high-temperature properties.

In addition, since the PCS fiber bundle must be subjected to chemical treatment after going through the process of winding and rewinding the PCS fiber bundle, there is a problem that the time and cost required for the overall SiC fiber manufacturing process are greatly increased.

The present invention is to solve the above problems, and an object of the present invention is to enable a continuous process to the infusible treatment (chemical treatment) process of the PCS fiber after the melt spinning process of the polymer PCS, and to prevent damage or disconnection of the fiber. It is to provide a device for preventing continuous infusible of PCS fibers and a method for infusible thereof. However, these problems are exemplary, and the scope of the present invention is not limited thereby.

A device for continuously infusible PCS fibers according to an embodiment of the present invention includes: a guide tube connected to one side of a melt spinning unit and guiding the PCS fibers melt-spun from the melt spinning unit; And a heating unit that applies heat to the PCS fibers in the guide tube, wherein curing gas is injected and discharged inside the guide tube, and the heating unit comprises a heating element surrounding the guide tube and the heating element. It may be provided with an enclosing reflector.

In addition, in the device for continuously infusible PCS fibers according to an embodiment of the present invention, the guide tube may be made of a transparent ceramic material.

In addition, in the device for continuous incompatibility of PCS fibers according to an embodiment of the present invention, the heating unit may be configured in plural and disposed to be spaced apart along the length direction of the guide tube.

In addition, in the device for continuous infusion of PCS fibers according to an embodiment of the present invention, the heating unit may have a toroid shape.

In addition, in the device for continuous incompatibility of PCS fibers according to an embodiment of the present invention, the guide tube may have a curing gas injection line connected to one side and a curing gas discharge line connected to the other side.

In addition, in the device for continuously infusible PCS fibers according to an embodiment of the present invention, a winder for winding the infusible PCS fibers to the other side of the guide tube may be connected.

In addition, the device for continuous incompatibility of PCS fibers according to an embodiment of the present invention may select any one of oxidation curing and chemical vapor curing.

In addition, a method for continuously infusible PCS fibers according to an embodiment of the present invention includes: guiding the PCS fibers melt-spun from the melt-spinning unit by a guide tube connected to one side of the melt-spinning unit; And applying heat by a heating unit including a heating element surrounding the guide tube and a reflecting plate surrounding the heating element to apply heat to the PCS fiber in the guide tube, wherein the curing gas is injected and discharged inside the guide tube. Can be done.

In addition, the continuous infusible method of PCS fibers according to an embodiment of the present invention may use the PCS continuous infusible device of the present invention.

According to an embodiment of the present invention made as described above, the continuous infusible device of PCS fibers continuously undergoes chemical treatment (infusible treatment) without separately winding and rewinding the melt-spun PCS fibers, The manufacturing process of the SiC fiber becomes simpler, and the manufacturing time can be drastically shortened. That is, it is possible to omit the process of winding and rewinding the fibers between the melt spinning process and the curing (infusible) process. In addition, since the PCS fiber can be stably obtained without breakage or disconnection by omitting the winding process, the mechanical properties of the finally produced SiC fiber can be remarkably improved. In addition, since the spun PCS fiber is immediately cured, it is possible to more easily handle the PCS fiber, and since the process is performed continuously, process time and cost can be saved. Of course, the scope of the present invention is not limited by these effects.

1 is a diagram schematically showing a device for continuous infusible of PCS fibers.
Fig. 2 is an overall perspective view of a continuous infusible device of PCS fibers.
3 is a partially enlarged view of a continuous infusible device of PCS fibers.
4 is a partial cross-sectional view of a continuous infusible device of PCS fibers.
5 is a diagram showing a curing (infusible treatment) process of a continuous infusible device of PCS fibers.
6 is a SEM-EDS analysis table before and after application of continuous incompatibility.
7 is a photograph of PCS fibers and SiC fibers.

Objects, features, and advantages of the present invention described above will become more apparent through the following embodiments in connection with the accompanying drawings.

The following specific structure or functional descriptions are exemplified only for the purpose of describing embodiments according to the concept of the present invention, and embodiments according to the concept of the present invention may be implemented in various forms and described in the present specification or application. It should not be construed as being limited to the examples.

Since embodiments according to the concept of the present invention can be modified in various ways and have various forms, specific embodiments are illustrated in the drawings and will be described in detail in the present specification or application. However, this is not intended to limit the embodiments according to the concept of the present invention to a specific form of disclosure, and should be understood to include all changes, equivalents, and substitutes included in the spirit and scope of the present invention.

Terms such as first and/or second may be used to describe various elements, but the elements are not limited to the terms. The above terms are only for the purpose of distinguishing one component from other components, for example, without departing from the scope of the rights according to the concept of the present invention, the first component can be named as the second component, and is similar. Thus, the second component may also be referred to as a first component.

When a component is referred to as "connected" or "connected" to another component, it may be directly connected or connected to the other component, but other components may exist in the middle. It should be understood. On the other hand, when a certain component is referred to as "directly connected" or "directly connected" to another component, it should be understood that no other component exists in the middle. Other expressions for describing the relationship between the constituent elements, such as "between" and "directly between" or "adjacent to" and "directly adjacent to" should be interpreted as well.

The terms used in this specification are only used to describe specific embodiments, and are not intended to limit the present invention. Singular expressions include plural expressions unless the context clearly indicates otherwise. In the present specification, terms such as "comprise" or "have" are intended to designate the existence of the described feature, number, step, action, component, part, or combination thereof, but one or more other features or numbers, It is to be understood that the presence or addition of steps, actions, components, parts, or combinations thereof does not preclude the possibility of preliminary exclusion.

Unless otherwise defined, all terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs. Terms as defined in a commonly used dictionary should be construed as having a meaning consistent with the meaning of the related technology, and should not be interpreted as an ideal or excessively formal meaning unless explicitly defined in the present specification. Does not.

Hereinafter, the present invention will be described in detail by describing a preferred embodiment of the present invention with reference to the accompanying drawings. The same reference numerals shown in each drawing indicate the same members.

Hereinafter, embodiments of the present invention will be described in more detail with reference to the drawings.

1 is a diagram showing a schematic view of a continuous infusible device of PCS fibers; Fig. 2 is a diagram showing the overall appearance of a continuous infusible device of PCS fibers; 3 is a partially enlarged view of a continuous infusible device of PCS fibers; 4 is a partial cross-sectional view of a continuous infusible device of PCS fibers; 5 is a cross-sectional view showing a curing (infusible treatment) process of a continuous infusible device of PCS fibers.

The continuous infusible device 100 of PCS fibers according to an embodiment of the present invention may include a guide tube 120 and a heating unit 130 connected to one side of the melt spinning unit 110. In addition, the continuous infusible device 100 of the PCS fiber may optionally further include a melt spinning unit 110.

The melt spinning unit may form a yarn by heating and melting a material polymer, and extruding the molten material through a nozzle while applying pneumatic pressure to cool and solidify the material. The melt spinning unit 110 may include a raw material melting tank 111, a raw material melting tank heater 112, and a melt spinning nozzle 114, as shown in FIGS. 1, 3, and 4. . The raw material melting tank 111 may store the raw material M. That is, a raw material, for example, a lump-shaped PCS may be built into the raw material melting tank 111. The raw material melting tank 111 may be made of stainless steel. However, the present invention is not limited thereto, and a material having a heat-resistant temperature of about 500° C. and having good chemical resistance that does not react with a material such as PCS is preferable. The heater 112 for the raw material melting tank may be disposed around the raw material melting tank and heated in order to melt the PCS. In addition, the melt spinning nozzle 114 may extrude the melted PCS. The raw material M (eg, PCS in a lump shape) may be converted into yarn (eg, PCS fibers) by being extruded through the melt spinning nozzle 130. That is, a melt spinning process is performed.

Since such a melt spinning process melts the PCS at a temperature near the melting point of the PCS, it must be performed under the influence of an inert atmosphere to prevent the PCS from being oxidized at the melting temperature. In order to create an inert atmosphere, an inert gas injection line 420 may be connected to the melt spinning unit. That is, an inert gas, for example, nitrogen, argon, carbon dioxide, etc. may be injected through the inert gas injection line. Further, in order to form an inert atmosphere, a mixed gas may be used. The mixed gas may be introduced from the gas mixer 300 to the melt spinning unit through the inert gas injection line 420. The mixed gas may be, for example, a mixed gas of nitrogen and oxygen, argon and oxygen, and ozone and oxygen. In addition, in order to form an inert atmosphere, a stopper 113 may be formed on the top of the raw material melting tank 111.

In addition, in the melt spinning process, when PCS reacts with oxygen, oxidation curing takes place in advance, so that the PCS is hardened without melting. Accordingly, in order to remove air from the inside of the raw material melting tank, a vacuum pump 200 and a pump line 410 connected from the vacuum pump 200 may be provided. The pump line 410 may be connected to the melt spinning unit 110.

On the other hand, PCS is decomposed by a heat treatment process at a high temperature (for example, at least about 1000°C) and is converted from a polymer to SiC, a ceramic. In case of heat treatment of non-cured PCS at high temperature, PCS swells or melts because most of the PCS is decomposed in a gaseous form with a ceramic yield of about 50 to 55%. Therefore, the curing (infusible) process corresponds to an essential process for converting PCS fibers into ceramic fibers. In the curing process, a thermoplastic polymer is converted into a thermosetting polymer through a chemical reaction, and a low molecular weight polymer unit is made into a larger unit through a crosslinking or radical bonding. The guide tube 120 and the heating unit 130 in which such a curing process is performed will be described as follows.

1 to 4, the guide tube 120 may be connected to the melt spinning unit 110. That is, after the melt spinning process of the PCS, the curing (infusible treatment) process may be continuously performed. Accordingly, compared to the prior art, the continuous infusible device 100 of PCS fibers according to the present invention allows continuous curing (infusible treatment) without separately winding and rewinding the melt-spun PCS fibers. . Accordingly, it is possible to chemically treat PCS fibers without breakage or disconnection, and heat treatment of such PCS fibers to produce high-quality SiC fibers. In addition, due to the above-described continuous process, the SiC fiber manufacturing process can be simplified, and manufacturing time and cost can be greatly reduced.

The guide tube 120 is preferably connected to the lower end of the melt spinning unit, but is not limited thereto. In addition, the guide tube 120 and the melt spinning unit 110 may be directly connected, but a separate focusing device (not shown) may be provided between the guide tube 120 and the melt spinning unit 110 have. When a focusing device is provided, hundreds of PCS fibers can be bundled and chemically treated (infusible treatment) continuously. In addition, a separate winder (not shown) may be connected to the other side of the guide tube 120 to wind the cured (infusible) PCS fiber. After winding the PCS fiber in which melt spinning and curing (incompatibility) have been continuously performed, the wound fiber may be released again to perform a heat treatment process.

In addition, according to an embodiment of the present invention, the guide tube 120 may guide the melt-spun PCS fiber to be cured (infusible treatment). In particular, it may be guided to pass through the heating unit 130 to be described later. In addition, when the very thin PCS fiber is melt-spun and cured, it may be affected by an external force, and the guide tube 120 can minimize this external influence. For example, the guide tube 120 may prevent the PCS fiber from being shaken by the wind, the nozzle being cooled down quickly, and the like.

The guide tube 120 may be made of a ceramic material, for example, quartz, high temperature glass, or the like. In addition, the guide tube 120 may be made of a transparent material so as to check the movement of the melt-spun PCS fibers inside. However, it is not limited thereto.

For the curing process, since it is necessary to convert the thermoplastic polymer into a thermosetting polymer through a chemical reaction, the process must be performed under the influence of various atmospheres. That is, a curing gas (eg, oxygen, iodine, etc.) is injected and/or discharged into the guide tube 120, and a curing atmosphere must be created. In order to control the atmosphere of the guide tube 120, a curing gas injection line 510 on one side of the guide tube 120 and a curing gas discharge line 520 on the other side may be disposed.

Meanwhile, the curing process of PCS can be divided into oxidation curing and chemical vapor curing. Oxidation curing using oxygen as a crosslinking agent is performed at about 150°C or higher, and the higher the reaction temperature, the higher the oxygen diffusion rate into the PCS fiber, so the process time can be shortened. Chemical vapor curing is cured by chemically reacting a crosslinking agent such as iodine or cyclohexane in a gaseous phase. Compared with oxidation curing, the gas used for chemical vapor curing has a disadvantage in that it is toxic, but has the advantage of reducing process cost because it has a fast reaction rate at a low temperature.

The continuous infusible device 100 of PCS fibers according to an embodiment of the present invention may select oxidation curing or chemical vapor curing. That is, by selecting a curing (insoluble) gas injected and/or discharged into the guide tube 120, a curing method may be selected. For example, when oxidizing curing is used, the inside of the guide tube 120 may be formed in an oxygen atmosphere, and when chemical vapor curing is used, the inside of the guide tube 120 may be formed in an iodine atmosphere. In addition, when a mixed gas is used during the curing process, the gas mixer 300 may be used.

In addition, as shown in FIG. 5, the curing (infusible) gas may have a traveling direction 30 flowing from one side to the other while surrounding the PCS fiber. For example, the curing gas is injected and/or discharged into the guide tube 120, and the flow of gas due to the injection and discharge of the curing gas helps the guide tube 120 guide the PCS fiber. May be. However, FIG. 5 is exemplary, and the flow of gas is not limited thereto, and it is sufficient to create an atmosphere in which curing can be performed.

Further, in the continuous infusible device 100 of PCS fibers according to the present invention, the heating unit 130 may include a heating element 131 and a reflecting plate 132. The heating element 131 may surround the guide tube 120, and the reflector 132 may surround the heating element 131. In order to achieve a crosslinking reaction in the PCS fiber, the heating unit 130 may apply heat to the PCS fiber guided along the guide tube 120. The heating element 131 and the reflector 132 may have a toroid shape. The reflective plate 132 is preferably made of a metal, but is not limited thereto.

As shown in FIG. 5, the reflective plate 132 may allow the heat of the heating element 131 to be concentrated on the PCS fiber inside the guide tube 120. For example, the heating element 131 may be an infrared lamp, and the infrared ray 40 emitted from the infrared lamp is reflected by colliding with the inner circumferential surface of the reflector 132, and the reflected infrared ray is inside the guide tube 120 Can be concentrated with PCS fibers.

In addition, the heating unit 130 may be configured in plural. A plurality of heating units may be disposed to be spaced apart along the length direction of the guide tube 120. For example, the heating units 130 may be provided in about 1 to 100 units and may be spaced apart from each other at regular intervals. However, this arrangement is exemplary, and a location capable of appropriately applying heat to the PCS fiber is sufficient.

By this incompatibility treatment, the thermoplastic PCS fiber is converted to thermosetting, so that even if the temperature is raised above the softening temperature and melting temperature in the subsequent pyrolysis process, it is possible to form SiC fibers that do not soften or melt and maintain the fiber shape as it is. And, at the same time, the pyrolysis yield can be improved.

6 shows the SEM-EDS analysis table before and after application of continuous incompatibility. It was found that oxygen was not included in PCS as shown in FIG. 6(a) before the oxidation curing process, whereas oxygen was included as shown in FIG. 6(b) after the oxidation curing process. I can. As a result of EDS, if more than 5wt% of oxygen is added through curing, it can be converted into SiC fibers.

7 shows PCS fibers and SiC fibers. Figure 7 (a) shows a state that the spinning and curing continuously proceeded PCS fibers are wound through a winder, and Figure 7 (b) shows a state that the PCS fibers are collected from the winder. 7C shows SiC fibers obtained by heat-treating the cured PCS fibers.

In addition, a support frame 10 for supporting the continuous infusible device 100 of PCS fibers according to the present invention may be installed. The support frame 10 may be formed as a table-shaped frame, as shown in FIGS. 1 and 2. In addition, the support frame 10 may include a raw material tank support 11 supporting the raw material tank and a reflecting plate support 12 supporting a reflecting plate of the heating unit. However, the present invention is not limited thereto, and may be formed in various shapes.

Next, a description will be given of a method of continuous incompatibility of PCS fibers according to an embodiment of the present invention.

In order to make the PCS into SiC fibers, the step of melt-spinning the lump-shaped PCS (S10), the step of curing the melt-spun PCS fiber (infusible treatment) (S20), and the step of heat-treating the cured PCS fiber ( S30) can be passed. In particular, according to an embodiment of the present invention, the melt spinning step (S10) and the curing step (S20) may be performed continuously. The curing step (S20), that is, the continuous infusion method of the PCS fiber according to the present invention, the guide tube 120 connected to one side of the melt spinning unit 110 is melt-spun PCS from the melt spinning unit 110 Guiding the fibers (S21); And applying heat to the PCS fiber in the guide tube 120 by the heating unit 130 having a heating element 131 surrounding the guide tube and a reflecting plate 132 surrounding the heating element (S22). can do. In the inside of the guide tube 120, for example, through the curing gas injection line 510 and/or the curing gas discharge line 520, the curing gas may be injected and discharged. When the PCS fiber subjected to the curing step (S20) is heat-treated (S30) at a high temperature in an inert atmosphere, a SiC fiber can be finally obtained.

The present invention has been described with reference to the embodiments shown in the drawings, but these are only exemplary, and those of ordinary skill in the art will understand that various modifications and equivalent other embodiments are possible therefrom. will be. Therefore, the true technical protection scope of the present invention should be determined by the technical spirit of the appended claims.

100: continuous infusible device of PCS fiber
110: melt spinning unit
120: guide tube
130: heating unit
111: raw material melting tank
112: heater for raw material melting tank
113: plug
114: melt spinning nozzle
131: heating element
132: reflector
510: curing gas injection line
520: curing gas discharge line

Claims (9)

A guide tube 120 connected to one side of the melt spinning unit 110 and guiding the PCS fibers melt-spun from the melt spinning unit 110; And
It includes a heating unit 130 for applying heat to the PCS fiber in the guide tube 120,
In the inside of the guide tube, the curing gas is injected and discharged,
The heating unit includes a heating element 131 surrounding the guide tube and a reflecting plate 132 surrounding the heating element.
Device for continuous incompatibility of PCS fibers.
The method of claim 1,
The guide tube 120 is made of a transparent ceramic material
Device for continuous incompatibility of PCS fibers.
The method of claim 1,
The heating unit 130 is composed of a plurality and is disposed to be spaced apart along the length direction of the guide tube.
Device for continuous incompatibility of PCS fibers.
The method of claim 1,
The heating unit 130 has a toroid shape
Device for continuous incompatibility of PCS fibers.
The method of claim 1,
The guide tube 120 has a curing gas injection line 510 connected to one side and a curing gas discharge line 520 connected to the other side.
Device for continuous incompatibility of PCS fibers.
The method of claim 1,
To the other side of the guide tube 120 is connected to a winder for winding the infused PCS fiber
Device for continuous incompatibility of PCS fibers.
The method of claim 1,
You can choose between oxidation curing and chemical vapor curing.
Device for continuous incompatibility of PCS fibers.
In the continuous infusible method of PCS fiber,
Guiding the PCS fibers melt-spun from the melt-spinning unit 110 by a guide tube 120 connected to one side of the melt-spinning unit 110; And
The heating unit 130 having a heating element 131 surrounding the guide tube 120 and a reflecting plate 132 surrounding the heating element includes applying heat to the PCS fiber in the guide tube,
In the guide tube 120, the curing gas is injected and discharged.
Method of continuous incompatibility of PCS fibers.
In the continuous infusible method of PCS fiber,
Using the continuous infusible device 100 of the PCS fiber of any one of claims 1 to 6
Method of continuous incompatibility of PCS fibers.

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