WO2019117473A1 - Sioic fiber, metal-doped sioic fiber, microwave absorption and heating element comprising same metal-doped sioic fiber, and manufacturing method therefor - Google Patents

Abstract

An embodiment of the present invention pertains to a SiOIC fiber comprising 30-50 % by weight of silicon(Si), 5-15 % by weight of oxygen (O), 3-15 % by weight of iodine (I), and 20-50 % by weight of carbon (C), a metal-doped SiOIC fiber comprising 3-30 % by weight of silicon (Si), 3-40 % by weight of oxygen (O), 5-50 % by weight of iodine (I), 5-40 % by weight of carbon (C), and 5-50 % by weight of a metal, a microwave absorption and heating element comprising the same metal-doped SiOIC fiber, and a manufacturing method therefor. According to the present invention, heating efficiency in response to microwaves can be remarkably increased and simultaneously, a remarkable improvement of durability can be brought about in the heating element by preventing or minimizing an oxygen-induced oxidative reaction.

Description

SIOIC fiber and metal doping SIOIC fiber, microwave absorbing and heating element containing it, and manufacturing method thereof

More particularly, the present invention relates to a SiOIC fiber and a metal-doped SiOIC fiber having excellent durability due to oxidation prevention or minimization of oxidation even under an oxygen atmosphere, And a method of manufacturing the microwave absorbing and heating element.

Microwave heating is a method of heating an object using microwave electromagnetic radiation. When a high frequency hits an object, the molecular dipole constituting the object quickly changes the direction of its axis by the high frequency electric field. Heat is generated. Generally, the microwaves used in the home microwave heating are 2.45 GHz or 915 MHz microwave.

The heating technology using microwave is clean because it does not use fossil fuel, and the heat conversion efficiency of the energy to be injected at the same time is high, so that rapid heat transfer, quick response speed and miniaturization can be achieved. Therefore, not only a lot of energy is consumed to increase the temperature at a high temperature, but also a heating method using an existing fossil fuel having a slow cooling rate after a high temperature heating or a heating method using an electric resistance Heating technology has been replaced by the trend.

Typically, SiC is used as a material to be heated by using microwaves. In general, a massive SiC block is processed into a heating body. However, since a heating element made of a SiC block has a large thickness and is heavy in weight, the heating rate to a high temperature of 1000 ° C or higher is not so fast and energy efficiency is not high. Also, because of the large weight, the cooling rate after the high temperature heat is not fast, so the working time can not be shortened remarkably.

Accordingly, efforts have been made to use conductive ceramic fibers capable of absorbing microwaves for microwave heating. As a typical conductive ceramic fiber, carbon fiber is exemplified. When a microwave of 2.45 GHz is irradiated, the conductive ceramic fiber exhibits a property of heating up to more than 1000 ° C and up to 2000 ° C in a few seconds. This is due to the fact that the heat generated by the microwaves rapidly radiates out of the fiber in proportion to the specific heat capacity, which is the thermal energy required to increase the material temperature of the unit mass by one degree, due to the thin diameter of the conductive ceramic fiber and the light weight thereof .

However, most of the heating elements using microwaves are heated with air in the presence of oxygen. However, in the case of carbon fiber, since oxidation starts from 480 ° C in the heating process, it can not be suitably used for heating at high temperature.

In addition to carbon fiber, other conductive ceramic fibers include SiC fibers, and SiC fibers have semiconductor electrical characteristics, so that the heating temperature and heat generation rate by microwaves are not so high.

In order to solve these problems of SiC fibers, attempts have been made to use metal powder as a heating element by adding SiC fibers during the manufacturing process. However, since SiC fibers are difficult to pass through the nozzle during the spinning process for fiberization, There was a difficult problem.

In addition, a method for improving the heat generation efficiency by microwave using SiC fiber having a carbon coating formed by coating carbon having excellent electrical conductivity on SiC fiber has been proposed (Patent Document 1). The method disclosed in Patent Document 1 is advantageous in that the SiC fiber is manufactured in the shape of a heating body and then carbon coating is performed, thereby simplifying the process relatively. However, the SiC fiber heating body having such a carbon coating has disadvantages of the conventional carbon fiber. That is, since the environment for use as a heating element is in the air in which oxygen exists, the carbon coating layer is oxidized and disappears at a temperature of 480 ° C or more like the carbon fiber, so that there is a serious problem in the durability of the heating element.

 Patent Document 1: Korean Patent No. 10-1745422 (June 27, 2017)

A problem to be solved by the present invention is to provide a microwave oven which absorbs microwaves and rapidly generates joule heat after eddy current is generated, thereby exhibiting excellent heat generating efficiency and at the same time preventing or minimizing oxidation reaction by oxygen, And a metal-doped SiOIC fiber, a microwave absorbing and heating element including the same, and a method of manufacturing the same.

One embodiment of the present invention for solving the above problems is a method of manufacturing a semiconductor device comprising 30 to 50 wt% of silicon (Si), 5 to 15 wt% of oxygen (O), 3 to 15 wt% of iodine (I) To 50% by weight of the composition.

In this embodiment, the SiOIC fibers may include one or more selected from β-SiC, SiO _2, graphene, SiI, SiCI, the group consisting of CIO SiOCI and crystal phase.

Another embodiment of the present invention is a method of manufacturing a semiconductor device comprising 3 to 30 wt% of silicon (Si), 3 to 40 wt% of oxygen (O), 5 to 50 wt% of iodine (I) % Of metal and 5 to 50 wt% of metal.

In this embodiment, the metal may be selected from the group consisting of titanium, iron, zirconium, aluminum, and combinations thereof. The SiOIC fiber be able to include at least one selected from β-SiC, SiO _2, graphene, SiI, SiCI, SiOCI, CIO , the group consisting of MI, MOI and MCI crystal phase, M can represent a metal .

Further, another embodiment of the present invention relates to a microwave absorbing and heating element including the SiOIC fiber according to the above embodiment.

According to another embodiment of the present invention, there is also provided a method of manufacturing a semiconductor device, comprising: mixing a polycarbosilane (PCS) solution and an iodine solution to form a gel mixture; Vacuum drying the mixture to form a solid phase mixture; Melt spinning the solid phase mixture to form mixed fibers; Reacting the mixed fibers with an iodine gas to thereby infiltrate the mixed fibers and infiltrating iodine into the mixed fibers; And thermally decomposing the mixed fibers under an inert atmosphere.

In this embodiment, the amount of iodine in the iodine solution may be in the range of 0.001 to 0.02 times the weight of the polycarbosilane contained in the polycarbosilane solution, and the amount of solvent is 10 to 50 times the weight of iodine Lt; / RTI > The amount of solvent in the polycarbosilane solution may range from 1 to 4 times the weight of the polycarbosilane. The step of mixing the polycarbosilane (PCS) solution and the iodine solution to form a gel-state mixture may be performed by mixing the polycarbosilane solution and the iodine solution, stirring the mixture at 50 to 100 ° C for 1 to 12 ≪ / RTI > for a period of time. The iodine gas may be gasified by exposing the solid phase iodine to a temperature of 100 to 200 ° C, and the solid phase iodine may be used in an amount of 0.1 to 1 times the weight of the mixture fiber.

In yet another embodiment of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: mixing a polycarbosilane (PCS) solution, an iodine solution, and a metal alkoxide solution to form a gel mixture; Vacuum drying the mixture to form a solid phase mixture; Melt spinning the solid phase mixture to form mixed fibers; Reacting the mixed fibers with an iodine gas to thereby infiltrate the mixed fibers and infiltrating iodine into the mixed fibers; And thermally decomposing the mixed fibers under an inert atmosphere. The step of thermally decomposing the mixture fiber reacted with the iodine gas under an inert atmosphere may include thermally treating the mixture fiber reacted with the iodine gas in a mold at a temperature of 900 to 1350 ° C.

In this embodiment, the metal alkoxide solution is selected from the group consisting of titanium isopropoxide, iron acetylacetonate, zirconium isopropoxide, aluminum acetylacetonate, and combinations thereof ≪ / RTI > and at least one metal alkoxide selected from the group consisting of < RTI ID = 0.0 > The amount of the metal alkoxide in the metal alkoxide solution may be in the range of 0.001 to 0.02 times the weight of the polycarbosilane, and the amount of the solvent may be in the range of 50 to 100 times the weight of the metal alkoxide. The amount of iodine in the iodine solution may be in the range of 0.001 to 0.02 times the weight of the polycarbosilane contained in the polycarbosilane solution and the amount of the solvent may be in the range of 10 to 50 times the weight of the iodine . The amount of solvent in the polycarbosilane solution may range from 1 to 4 times the weight of the polycarbosilane. The step of mixing the polycarbosilane (PCS) solution and the iodine solution to form a gel-state mixture may be performed by mixing the polycarbosilane solution and the iodine solution, stirring the mixture at 50 to 100 ° C for 1 to 12 ≪ / RTI > for a period of time. The iodine gas may be gasified by exposing the solid phase iodine to a temperature of 100 to 200 ° C, and the solid phase iodine may be used in an amount of 0.1 to 1 times the weight of the mixture fiber. The step of thermally decomposing the mixture fiber reacted with the iodine gas under an inert atmosphere may include thermally treating the mixture fiber reacted with the iodine gas in a mold at a temperature of 900 to 1350 ° C.

The SiOIC fiber and the metal-doped SiOIC fiber according to the present invention can generate heat up to a temperature of 1000 ° C. or higher and a maximum of 1600 ° C. within a few seconds by microwave irradiation. In the absence of a carbon coating, The oxidation is hardly occurred and the durability is very excellent.

Accordingly, since the microwave heating element using the SiOIC fiber and the metal-doped SiOIC fiber is formed into a fibrous shape, the heat radiation efficiency to the outside is high, and the energy efficiency can be remarkably improved.

In addition, according to the present invention, since the fibers that have been irradiated and then incompatible with each other are put into various molds and heat-treated to produce SiOIC fibers and metal-doped SiOIC fibers, various shapes of heating elements can be easily manufactured. Accordingly, the microwave heating body having various shapes thus manufactured can be effectively applied to various fields such as a heat exchanger for a farm, a household, and an industrial use, a heating coil for a hot tower, a cook top,

In addition, according to the present invention, metal-doped SiOIC fibers having various functions such as catalytic properties can be produced by doping various kinds of metal with SiOIC fibers. Such metal-doped SiOIC fibers exhibit further improved heat- The requirements can be met.

1 is a SEM photograph of a SiC fiber according to the prior art.

2 is a SEM photograph of a SiOIC fiber according to an embodiment of the present invention.

Figures 3a and 3b are SEM photographs of Ti doped SiOIC fibers according to another embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings, so that those skilled in the art can easily carry out the technical idea of the present invention. In the following description, numerous specific details are set forth, such as specific elements, which are provided to aid a more thorough understanding of the present invention, and it is to be understood that the present invention may be practiced without these specific details, It will be obvious to those who have. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.

Conventionally, amorphous SiC fibers are prepared by heat treating polycrystalline polycarbosilane (PCS) fibers, which have undergone oxygen stabilization through an oxygen-stabilized atmosphere, at a temperature of 1350 ° C or lower. For example, they include 38.17 to 54.61% ) 31.27 to 40.18% by weight and oxygen (O) 14.12 to 21.65% by weight. The crystalline phase of the amorphous SiC fiber can be composed of nano-sized β-SiC, nano-sized SiO ₂ , graphene, and the like. These SiC fibers have semiconductor electrical characteristics, so that the heating temperature and heat generation rate by microwave irradiation are not so high.

An embodiment of the present invention is to provide a SiOIC fiber and a metal-doped SiOIC fiber having a new composition different from that of the conventional amorphous SiC fiber, exhibiting excellent heating efficiency by microwave irradiation, excellent oxidation stability, and improved durability.

The SiOIC fiber according to one embodiment of the present invention comprises 30 to 50% by weight of silicon (Si), 5 to 15% by weight of oxygen (O), 3 to 15% by weight of iodine (I) Preferably from 34 to 49% by weight of silicon (Si), from 9 to 13% by weight of oxygen (O), from 5 to 12% by weight of iodine (I) and from 25 to 50% by weight of carbon (C) % ≪ / RTI > by weight. These SiOIC fibers effectively contain iodine, which affects the electrical conductivity and current generation inside the fiber, thereby significantly improving the heat efficiency corresponding to the irradiation of the microwave.

According to another embodiment of the present invention, the metal-doped SiOIC fiber comprises 3 to 30 wt% of silicon (Si), 3 to 40 wt% of oxygen (O), 5 to 50 wt% of iodine (I) (I) 6 to 40% by weight of oxygen (C), 5 to 40% by weight of a metal and 5 to 50% by weight of a metal, preferably 5 to 25% To 47 wt%, carbon (C) 7 to 35 wt%, and metal 7 to 48 wt%. Such a metal-doped SiOIC fiber effectively contains the metal element in the fiber in addition to the iodine, thereby exerting a positive effect on the heat-generating behavior corresponding to the irradiation with the microwave, thereby further improving the heat-generating efficiency.

The SiOIC fiber and the metal-doped SiOIC fiber having the new composition can exhibit a high heat generation performance in a few seconds by heating up to a temperature of more than 1000 ° C. and a maximum of 1600 ° C. by the microwave irradiation. At the same time, The oxidation hardly occurs and the durability can be remarkably improved.

SiOIC fiber according to the embodiment may include at least one selected from β-SiC, SiO _2, graphene, SiI, SiCI, the group consisting of SiOCI and CIO crystal phase, metal-doped SiOIC fibers, β-SiC, SiO ₂ , graphene, SiI, SiCI, SiOCI, CIO, MI, MOI, and MCI. M represents a doped metal.

The metal included in the metal doped SiOIC fibers may be selected from the group consisting of titanium, iron, zirconium, aluminum, and combinations thereof. By doping various metals into the SiOIC fiber, it is possible to further improve the heating efficiency corresponding to the microwave, to give various functions such as the catalyst characteristics, and to meet the individual characteristic requirements required in each application field.

The SiOIC fiber and the metal-doped SiOIC fiber may be formed into a shape randomly or isotropically arranged in a mold having various shapes according to a desired purpose after the radiation is completed, and heat-treated.

Another embodiment of the present invention relates to a microwave absorbing and heating element comprising a SiOIC fiber or a metal-doped SiOIC fiber according to the above embodiment. As described above, the microwave absorbing and heating element according to the embodiment of the present invention has high heat generating efficiency, high oxidation stability, excellent durability, can be easily manufactured in various forms, can be miniaturized, , And can exhibit environment-friendly characteristics.

According to another aspect of the present invention, there is provided a method of manufacturing a SiOIC fiber, comprising: mixing a polycarbosilane (PCS) solution and an iodine solution to form a gel-like mixture; Vacuum drying the gel-like mixture to form a solid phase mixture; Melt spinning the solid phase mixture to form blended fibers; Reacting the mixed fibers with an iodine gas, infusing the mixed fibers and infiltrating iodine into the fibers; And thermally decomposing the fiber into a mold and under an inert atmosphere.

First, the polycarbosilane solution and the iodine solution may be mixed to form a gel-like mixture.

The solvent used in the polycarbosilane solution may be one or more selected from the group consisting of alcohols, toluene, xylene, cyclohexane, and combinations thereof.

The amount of solvent in the polycarbosilane solution may range from 1 to 4 times the weight of the polycarbosilane. If the amount of the solvent is less than 1 time of the weight of the polycarbosilane, the polycarbosilane may not be completely dissolved. If the amount of the solvent is more than 4 times, the solubility of the polycarbosilane may not be increased.

The solvent used in the iodine solution may be one or more selected from the group consisting of alcohols, toluene, xylene, cyclohexane, and combinations thereof.

The amount of solvent in the iodine solution may range from 10 to 50 times the weight of iodine. If the amount of the solvent is less than 10 times the weight of the iodine, the iodine may not be completely dissolved. If the amount of the solvent is more than 50 times, the increase in the amount of the solvent is not expected to increase.

The amount of iodine in the iodine solution may range from 0.001 to 0.02 times the weight of the polycarbosilane contained in the mixed polycarbosilane solution. If the amount of iodine is less than 0.001 times the weight of the polycarbosilane, pyrolysis may occur during the heat treatment during the fiberization process in the subsequent process, so that the amount of iodine present in the fiber may be almost zero. The thermal inductivity of the mixture may deteriorate to such an extent that the fiber can not be formed in the drying process, so that the spinning may be difficult and the fiber shape may not be obtained.

By mixing the polycarbosilane solution with the iodine solution, the iodine may be contained in the fiber and remain in the doped state even after the heat treatment. By using iodine in a solution state, even a small amount of iodine can be sufficiently doped into the fiber, and the process is easy and safe.

To prepare the metal-doped SiOIC fibers, a mixture of a polycarbosilane solution and an iodine solution may be added to further mix the metal alkoxide solution.

In this embodiment, when the metal-doped SiOIC fiber is prepared, fibers are prepared by mixing a solution of a polycarbosilane as a raw material and a solution of a metal alkoxide containing a metal to be doped together with an iodine solution, It is possible to effectively dope the metal element in the SiOIC fiber.

The metal alkoxide solution includes an alkoxide of a metal to be doped and includes, for example, titanium isopropoxide, iron acetylacetonate, zirconium isopropoxide, aluminum acetyl One or more metal alkoxides selected from the group consisting of aluminum acetylacetonate and combinations thereof.

The solvent used in the metal alkoxide solution may be one or more selected from the group consisting of alcohols, toluene, xylene, cyclohexane, and combinations thereof.

The amount of solvent in the metal alkoxide solution may range from 50 to 100 times the weight of the metal alkoxide. If the amount of the solvent is less than 50 times the weight of the metal alkoxide, the concentration is too high and the mixing efficiency with the polycarbosilane solution and the iodine solution is not good. If the solvent is more than 100 times, no further uniform mixing effect will occur.

The amount of the metal alkoxide in the metal alkoxide solution may range from 0.001 to 0.02 times the weight of the polycarbosilane contained in the mixed polycarbosilane solution. If the amount of the metal alkoxide is less than 0.001 times the weight of the polycarbosilane, pyrolysis may occur during the heat treatment during the fiberization process in the subsequent process so that the amount of the metal element present in the fiber may be almost zero. If the amount is more than 0.02 times, And it is difficult to achieve uniform dispersion.

A polycarbosilane solution and an iodine solution; Or a mixture of a polycarbosilane solution, an iodine solution and a metal alkoxide solution, and then maintaining the mixture at 50 to 100 DEG C for 1 to 12 hours while stirring, to form a gel-like mixture.

If the temperature is less than 50 ° C, the drying efficiency is very low and the solvent drying time may be very slow. If the temperature exceeds 100 ° C, the mixed solution starts boiling and the process is difficult to proceed.

Next, the gel-state mixture can be vacuum dried to form a solid phase mixture.

Vacuum drying can be done under vacuum with a degree of vacuum in the range of several to 10 ^-2 torr. Vacuum drying can also be performed in a temperature range of 150 to 250 ° C. If the vacuum drying temperature is lower than 150 ° C, the drying effect is not exhibited. If the vacuum drying temperature is higher than 250 ° C, the gel-state mixed solution is cured and the subsequent fiberizing process by melt spinning can not proceed.

Next, the solid phase mixture can be melt spinned to form mixed fibers.

In one example, the fiber formation can be carried out by forming a solid mixture in an emissive block, introducing nitrogen gas or the like into the interior of the emitter block to form an inert atmosphere, heating the mixture at 200 to 300 캜 to melt the solid mixture, To increase the pressure inside the spinning block to allow the molten mixture to flow through the nozzle, and then to control the supply of a certain amount of molten mixture to the nozzle by the gear pump. Through this process, a fibrous mixture can be formed in the form of long fibers and short fibers.

When the temperature is lower than 200 ° C., the melt viscosity of the melted mixture is too high due to the relatively low temperature, so that the melt can not be efficiently injected into the nozzle, ° C., the viscosity of the molten mixture becomes too low due to an excessively high temperature, and flows like water, and no fibrosis is caused.

Next, the mixed fibers are allowed to react with the iodine gas, and the mixed fibers are subjected to an infusibilizing treatment to infiltrate the iodine into the mixed fibers.

The iodine gas can be obtained by gasifying the solid phase iodine by exposing it to a temperature of 100 to 200 ° C.

The solid phase iodine may be 0.1 to 1 times the weight of the mixed fibers to be reacted. When the amount of solid iodine is less than 0.1 times the weight of the mixed fiber, the insolubilization of the mixed fiber and the iodine penetration into the fiber are difficult to occur effectively. When the amount of solid iodine is more than 1 time, Iodine penetration effect is not increased.

By reacting the mixed fibers with the iodine gas, the mixed fibers are converted into thermosetting properties, and a large amount of iodine can be infiltrated into the mixed fibers. Thus, even if the temperature is increased above the softening temperature and the melting temperature in the subsequent pyrolysis step, the fibrous phase can be maintained without being softened or melted, and the pyrolysis yield can also be improved.

Next, the fiber which is incompatible and has iodine impregnated therein can be pyrolyzed in an inert atmosphere.

The fibers which are insoluble through pyrolysis and into which iodine is impregnated can be converted into ceramics and converted into SiOIC fibers or metal-doped SiOIC fibers.

The pyrolysis can be carried out at a temperature of 900 to 1350 ° C. When the temperature is less than 900 ° C., the thermal decomposition of the fiber is not sufficiently performed, and the electrical and physical properties may be significantly deteriorated. When the temperature exceeds 1350 ° C., the thermal decomposition occurs sufficiently. However, The SiOIC fiber itself may decompose and lose its fiber shape and may change into a powder.

The pyrolysis process is incompatible and can be made with the fiber into which the iodine has penetrated into the mold. The frame may be selected according to the shape of the product to which the fiber is applied, for example, the microwave absorbing and heating element, and may be, for example, a circle, a rectangle, a square, or the like.

By the thermal cracking process in the mold, the SiOIC fiber or the metal doped SiOIC fiber can have a random or isotropically arranged shape.

In this embodiment, by forming the SiO 2 fiber and the metal-doped SiOIC fiber by thermally decomposing the unfused fiber in a mold, it can be easily applied to various shapes according to the product to be applied.

Hereinafter, the present invention will be described in more detail by way of examples. However, the following examples are illustrative of the present invention, and the scope of the present invention is not limited to the following examples.

[Example]

1. Manufacture of SiOIC fiber

(1) Production of polycarbosilane solution

After 30 g of toluene (30 ml) was added to the beaker, 10 g of solid polycarbosilane (manufactured by Tobiamec Co., Ltd., molecular weight Mw = 3500) was added and then magnetized on a hot plate for 12 hours to completely dissolve the solid polycarbosilane By performing stirring by means of a bar, a polycarbosilane solution was obtained.

(2) Preparation of iodine solution

To the beaker was added 3 g of toluene (3 ml), and 0.1 g of solid phase iodine (purchased from Samseon Pure Chemical Industries, Ltd., purity: 99.8%) was added. Then, on a hot plate for 12 hours to completely dissolve the solid phase iodine, By performing stirring by means of a bar, an iodine solution was prepared.

(3) Mixed solution formation

For the preparation of the SiOIC fibers, the polycarbosilane solution prepared above and the iodine solution were mixed and stirred by a magnetic bar on a hot plate for 10 hours. At this time, the temperature of the hot plate was maintained at 80 캜. The mixed solution was heated on a hot plate until the gel state became dry while the mixed solution was gelled, and the stirring was stopped when the viscosity of the mixed solution became higher and the magnetic bar no longer rotated.

(4) Vacuum drying

The gelled mixture was placed in a vacuum drier and the degree of vacuum inside the vacuum drier was adjusted to 8 x 10 ^-1 torr. The vacuum dryer temperature was adjusted to 180 DEG C and held for 10 hours to complete vacuum drying.

(5) Mixture fiber formation

5 g of the solid phase mixture formed by vacuum drying was placed in a radiator having one hole of 0.3 mm and the temperature of the radiation block was raised to 150 캜. In this case, the degree of vacuum inside the spinning block was about 3 × 10 ^-1 torr, and maintained at a temperature of 150 ° C. for 3 hours. Then, an inert atmosphere was formed by injecting nitrogen gas into the spinning block. The temperature was then increased to 210 < 0 > C and held for 2 hours. Subsequently, an inert gas was further injected to raise the pressure inside the spinning block to 0.01 MPa to allow the molten mixture to flow to the nozzle, and the molten mixture pushed to the end of the nozzle hole was stretched and wound on a winder to perform fiberization . The diameters of the prepared mixture fibers were about 20 to 25 탆.

(6) Disintegration of mixture fibers and penetration of iodine

The mixture fibers were placed in a graphite sieve and placed in a vacuum dryer. Then, 3 g of solid phase iodine was placed in the lower part of the graphite body placed in the vacuum dryer. Thereafter, the inside of the vacuum dryer was adjusted to a degree of vacuum of 5 x 10 < ^-1 > torr, and at the same time, the temperature was raised to 180 DEG C so that solid iodine in the graphite was gasified. The formed iodine gas actively reacted with the blend fibers to insolubilize the blend fibers and at the same time actively infiltrate the blend fibers with iodine. And kept at 180 ° C for 1 hour in a vacuum dryer equipped with a vacuum to complete the infiltration and penetration of iodine.

(7) Pyrolysis

1.5 g of the mixture fiber having incompatibility and iodine penetration was charged into a 50 mm diameter circular graphite mold and charged into an inert atmosphere. Nitrogen gas was injected into the furnace to form an inert atmosphere. The temperature was raised to 1350 占 폚 at a heating rate of 10 占 폚 / min, maintained at 1350 占 폚 for 1 hour, and then naturally cooled. The polymer fibers were pyrolyzed by heat treatment to obtain SiOIC fibers converted into ceramics.

2. Manufacture of metal doped SiOIC fibers

Doped SiOIC (silicon oxytitanium iodide) was prepared in the same manner as in (1) above except that the polycarbosilane solution and the iodine solution were further added with a metal alkoxide solution during the formation of the (3) Carbon) fiber.

The metal alkoxide solution was prepared by adding 3 g of toluene (3 ml) to a beaker, adding 0.04 g of titanium isopropoxide (purchased from Aldrich Korea, purity of 99.5%) and then dissolving the titanium isopropoxide in a hot plate ≪ / RTI > for 12 hours by means of a magnetic bar.

3. Results

(1) SEM photograph and elemental analysis of SiOIC fiber

FIG. 1 is a SEM photograph of a SiC fiber according to the prior art, and FIG. 2 is a SEM photograph of a SiOIC fiber according to an embodiment of the present invention. The results of elemental analysis measured at three spots shown in the SEM photographs of Figs. 1 and 2 are shown in Tables 1 and 2, respectively.

Spot No.		Si	C	O
One	wt%	38.17	40.18	21.65
	at%	22.43	55.23	22.34
2	wt%	42.54	36.83	20.63
	at%	25.8	52.23	21.97
3	wt%	54.61	31.27	14.12
	at%	35.80	47.94	16.26

As shown in Table 1, the SiC fibers according to the prior art shown in Fig. 1 are SiC fibers which have been infused with oxygen, and are composed of silicon (Si) 38.17 to 54.61 wt%, carbon (C) 31.27 to 40.18 wt % And oxygen (O) 14.12 to 21.65 wt%.

Spot No.		Si	C	O	I
One	wt%	42.39	38.95	9.53	9.13
	at%	27.85	59.84	10.99	1.32
2	wt%	34.37	49.2	10.84	5.59
	at%	20.25	67.8	11.22	0.73
3	wt%	48.36	27.69	12.51	11.44
	at%	35.14	47.05	15.96	1.85

As shown in Table 2, the SiOIC fibers according to an embodiment of the present invention shown in FIG. 2 were prepared by adding iodine, 34.37 to 48.36 wt% of silicon (Si), 27.69 to 49.2 wt% (O) 9.53 to 12.51 wt.%, And iodine (I) 5.59 to 11.44 wt.%. Figures 3a and 3b are SEM images of titanium doped SiOIC fibers according to another embodiment of the present invention, The elemental analysis results measured in the three spots shown in the SEM photographs of Figs. 3A and 3B are shown in Tables 3 and 4, respectively.

Spot No.		Si	C	O	Ti	I
P1	wt%	5.04	17.69	12.64	47.93	16.70
	at%	5.02	41.21	22.11	28.01	3.65
P2	wt%	16.93	28.70	28.66	10.38	15.33
	at%	11.77	46.65	34.99	4.23	2.36
P3	wt%	23.41	7.28	3.93	18.74	46.64
	at%	34.09	24.81	10.05	15.97	15.08

Spot No.		Si	C	O	Ti	I
P1	wt%	21.60	34.00	25.71	7.74	10.95
	at%	14.10	51.89	29.46	2.96	1.59
P2	wt%	14.72	29.19	36.93	12.42	6.74
	at%	9.40	43.59	41.40	4.65	0.96
P3	wt%	24.72	22.60	27.21	13.69	11.78
	at%	18.19	38.87	35.12	5.91	1.91

As shown in Tables 3 and 4, the titanium-doped SiOIC fibers according to another embodiment of the present invention include iodine and titanium, and include 5.04 to 24.72 wt% silicon (Si), 7.28 wt% (I) 6.74 to 46.64 weight%, and titanium 7.74 to 47.93 weight%. Thus, the SiOIC fibers according to the embodiments of the present invention have a composition of 34.00 wt%, oxygen (O) 3.93-36.93 wt%, iodine By including iodine in the fiber, which affects electrical conductivity and current generation, it can positively affect microwave-responsive exothermic behavior. In addition, the SiO ₂ fiber or the metal-doped SiOIC fiber according to the embodiment of the present invention has a lower oxygen content than that of the SiC fiber according to the related art, and the generation of SiO ₂ crystals is lowered, so that the electrical resistance can be lowered, .

(2) Heating performance

For comparison with the exothermic performance of the SiOIC fiber according to the embodiment, the microwave corresponding heat generation temperature of the amorphous SiC fiber according to the prior art is measured and shown in Table 5 below. The amorphous SiC fibers according to the prior art used in the experiments can be prepared according to methods known in the art, for example, polycondensation of polycarbosilane (PCS) fibers, which have undergone oxygen stabilization, in an inert atmosphere at 1350 DEG C Or less. The amorphous SiC fiber according to the related art may have a composition of, for example, 38.17 to 54.61% by weight of silicon (Si), 31.27 to 40.18% by weight of carbon (C) and 14.12 to 21.65% by weight of oxygen (O). The crystalline phase of the amorphous SiC fiber according to the prior art may be composed of nano-sized? -SiC, nano-sized SiO ₂ , graphene, or the like.

The prepared conventional SiC fiber was placed in a microwave irradiation chamber equipped with an infrared thermography camera (SDS HotFind DXS), and a microwave of 2.45 GHz was irradiated to irradiate the exothermic behavior generated by the SiC fiber by microwave interaction with infrared rays And analyzed with an infrared camera.

	Measurement result
Average temperature of the entire specimen	171 DEG C
Central part temperature	179 ° C
Maximum temperature	179 ° C
Minimum temperature	169 ° C
Standard Deviation	2.3 ℃
Temperature range	1.3%

As is known, the SiC fibers according to the prior art have a semiconductor electrical characteristic, so that there is a tendency that heat generation does not occur corresponding to microwaves. As can be seen in Table 5, the amorphous SiC fibers according to the prior art had maximum heat generation temperatures corresponding to microwaves of 179 ° C.

The heating temperature corresponding to the microwave of the SiOIC fiber according to the embodiment of the present invention manufactured in the above example was measured in the same manner as described above and is shown in Table 6 below.

	Measurement result
Average temperature of the entire specimen	1307 ℃
Central part temperature	1320 ° C
Maximum temperature	1320 ° C
Minimum temperature	1275 ℃
Standard Deviation	10.3 DEG C
Temperature range	0.8%

Referring to Table 6, it can be seen that the SiOIC fiber according to the embodiment of the present invention has a maximum heat of 1320 ° C corresponding to the microwave. This shows that the heating effect can be remarkably improved when the microwave irradiation is performed as compared with the amorphous SiC fiber according to the prior art shown in Table 5. [

The temperature of the Ti-doped SiOIC fiber according to another embodiment of the present invention was measured in the same manner as described above, and the results are shown in Table 7 below.

	Measurement result
Average temperature of the entire specimen	1598 ° C
Central part temperature	1602 DEG C
Maximum temperature	1602 DEG C
Minimum temperature	1549 ° C
Standard Deviation	12.6 ° C
Temperature range	0.8%

Referring to Table 7, Ti-doped SiOIC fibers according to an embodiment of the present invention include not only iodine but also metal elements in the fibers, and thus heat generation efficiency is further improved, .

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments or constructions. Various changes, substitutions and alterations can be made hereto without departing from the spirit and scope of the invention. It will be clear to those who have knowledge.

Claims (15)

1. A SiOIC fiber comprising 30 to 50 wt% silicon (Si), 5 to 15 wt% oxygen (O), 3 to 15 wt% iodine (I), and 20 to 50 wt% carbon (C).
2. The method according to claim 1,

   SiOIC said fibers comprising at least one selected from β-SiC, SiO _2, graphene, SiI, SiCI, the group consisting of a crystalline phase and CIO SiOCI

   SiOIC fiber.
3. 3 to 30 wt% of silicon (Si), 3 to 40 wt% of oxygen (O), 5 to 50 wt% of iodine, 5 to 40 wt% of carbon (C) and 5 to 50 wt% of metal Metal-doped SiOIC fibers.
4. The method of claim 3,

   Wherein the metal is selected from the group consisting of titanium, iron, zirconium, aluminum and combinations thereof

   Metal doped SiOIC fiber.
5. The method of claim 3,

   SiOIC the fiber comprises one or more selected from β-SiC, SiO _2, graphene, SiI, SiCI, SiOCI, CIO , the group consisting of MI, and MOI MCI crystal phase and, M is indicative of the metal

   Metal doped SiOIC fiber.
6. A microwave absorbing and heating element comprising the SiOIC fiber according to claim 1 or the metal doped SiOIC fiber according to claim 3.
7. Mixing a polycarbosilane (PCS) solution and an iodine solution to form a gel-like mixture;

   Vacuum drying the mixture to form a solid phase mixture;

   Melt spinning the solid phase mixture to form mixed fibers;

   Reacting the blended fibers with an iodine gas, infiltrating the blended fibers and infiltrating iodine into the blended fibers; And

   And thermally decomposing the mixture fiber reacted with the iodine gas under an inert atmosphere

   Method of making SiOIC fibers.
8. 8. The method of claim 7,

   The step of mixing the polycarbosilane (PCS) solution and the iodine solution to form a mixture comprises adding a metal alkoxide solution and mixing

   Method of making SiOIC fibers.
9. 9. The method of claim 8,

   The metal alkoxide solution may be selected from the group consisting of titanium isopropoxide, iron acetylacetonate, zirconium isopropoxide, aluminum acetylacetonate, and combinations thereof, wherein the metal alkoxide solution is selected from the group consisting of titanium isopropoxide, iron acetylacetonate, zirconium isopropoxide, aluminum acetylacetonate, RTI ID = 0.0 > metal alkoxide < / RTI >

   Method of making SiOIC fibers.
10. 9. The method of claim 8,

    The amount of the metal alkoxide in the metal alkoxide solution is in the range of 0.001 to 0.02 times the weight of the polycarbosilane and the amount of the solvent is in the range of 50 to 100 times the weight of the metal alkoxide

    Method of making SiOIC fibers.
11. 8. The method of claim 7,

    The amount of iodine in the iodine solution is in the range of 0.001 to 0.02 times the weight of the polycarbosilane contained in the polycarbosilane solution and the amount of the solvent is in the range of 10 to 50 times the weight of the iodine

    Method of making SiOIC fibers.
12. 8. The method of claim 7,

    The amount of solvent in the polycarbosilane solution is in the range of 1 to 4 times the weight of the polycarbosilane

    Method of making SiOIC fibers.
13. 8. The method of claim 7,

    The step of mixing the polycarbosilane (PCS) solution and the iodine solution to form a gel-state mixture may be performed by mixing the polycarbosilane solution and the iodine solution, stirring the mixture at 50 to 100 ° C for 1 to 12 ≪ / RTI > for a period of time.

    Method of making SiOIC fibers.
14. 8. The method of claim 7,

    The iodine gas is obtained by gasifying solid phase iodine at a temperature of 100 to 200 DEG C and the solid phase iodine is used in an amount of 0.1 to 1 times the weight of the fiber mixture

    Method of making SiOIC fibers.
15. 8. The method of claim 7,

    The step of thermally decomposing the mixture fiber reacted with the iodine gas under an inert atmosphere comprises heat-treating the mixture fiber reacted with the iodine gas in a mold at a temperature of 900 to 1350 ° C

    Method of making SiOIC fibers.

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