KR20050014033A - Preparation method of nano-porous carbon fibers through carbonization of electrospun nano-fibers - Google Patents
Preparation method of nano-porous carbon fibers through carbonization of electrospun nano-fibersInfo
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- KR20050014033A KR20050014033A KR1020050004575A KR20050004575A KR20050014033A KR 20050014033 A KR20050014033 A KR 20050014033A KR 1020050004575 A KR1020050004575 A KR 1020050004575A KR 20050004575 A KR20050004575 A KR 20050004575A KR 20050014033 A KR20050014033 A KR 20050014033A
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- activated carbon
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- nanofibers
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/1336—Illuminating devices
- G02F1/133615—Edge-illuminating devices, i.e. illuminating from the side
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/0001—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings specially adapted for lighting devices or systems
- G02B6/0011—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings specially adapted for lighting devices or systems the light guides being planar or of plate-like form
- G02B6/0013—Means for improving the coupling-in of light from the light source into the light guide
- G02B6/0023—Means for improving the coupling-in of light from the light source into the light guide provided by one optical element, or plurality thereof, placed between the light guide and the light source, or around the light source
- G02B6/0031—Reflecting element, sheet or layer
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/0001—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings specially adapted for lighting devices or systems
- G02B6/0011—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings specially adapted for lighting devices or systems the light guides being planar or of plate-like form
- G02B6/0033—Means for improving the coupling-out of light from the light guide
- G02B6/0058—Means for improving the coupling-out of light from the light guide varying in density, size, shape or depth along the light guide
- G02B6/0061—Means for improving the coupling-out of light from the light guide varying in density, size, shape or depth along the light guide to provide homogeneous light output intensity
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/133524—Light-guides, e.g. fibre-optic bundles, louvered or jalousie light-guides
Abstract
Description
본 발명은 활성화 공정을 거치지 않고 탄소화에 의해 나노세공분포를 갖는활성탄소나노섬유 부직포 제조에 관한 것이다.The present invention relates to the production of activated carbon nanofiber nonwoven fabric having nanopore distribution by carbonization without undergoing an activation process.
활성탄소섬유는 유기섬유를 방사한 후 산화안정화 처리하거나, 탄소화 및 산화안정화 처리된 섬유를 기체(스팀, CO2, 공기)와 무기화합물(ZnCl2, KOH, H3PO4) 등을 이용하여 섬유표면에 무수한 미세기공을 형성시키는 방법으로 제조된다.Activated carbon fiber is oxidative stabilized after spinning the organic fiber, or carbonized and oxidative stabilized fiber using gas (steam, CO 2 , air) and inorganic compounds (ZnCl 2 , KOH, H 3 PO 4 ) To form a myriad of micropores on the fiber surface.
상기 활성탄소섬유에 사용되는 전구체 재료로는 폴리아크릴로나이트릴(polyacrylonitrile, PAN), 셀룰로오스(cellulose), 피치(pitch), 페놀수지(phenol-resin) 등이 이용된다. 상기 재료를 용액방사나 용융방사에 의해 섬유를 제조한 다음, 고온 탄소화나 활성화 처리시 섬유의 융착이나 용융이 발생하지 않도록 산화안정화 처리한 다음, 이를 불활성 분위기하에서 500 - 1500℃ 온도 범위에서 탄소화 처리하여 탄소섬유를 제조한다.Precursor materials used in the activated carbon fibers include polyacrylonitrile (PAN), cellulose, pitch, phenol resin, and the like. The fibers are prepared by solution spinning or melt spinning, and then subjected to oxidative stabilization to prevent fusion or melting of fibers during high temperature carbonization or activation, and then carbonization at a temperature in the range of 500 to 1500 ° C. under an inert atmosphere. Treatment to produce carbon fibers.
제조된 안정화(불융화) 섬유나 탄소섬유는 산화성 기체나 각종 염류를 이용하여 700 - 1200 ℃ 온도범위에서 활성화하여 섬유표면에 무수한 미세공을 형성시키는 방법에 의해 활성탄소섬유가 제조되나, 이러한 방법은 제조공정상 에너지 낭비가 심하고, 세공구조를 제어하는데 제약이 있다. 특히 각종 염류를 이용한 약품활성화 방법은, 반응로(탄화로, 활성화로)의 부식과 함께 연속공정 및 대량생산에 어려움이 있으며, 사용전 산처리 및 중화처리를 하여 사용하는 불편함이 있다. 또한, 용액방사나 용융방사 방법으로 제조된 활성탄소섬유의 경우 직경이 10 - 20 ㎛ 범위가 대부분이어서 빠른 흡착, 탈착을 요구하는 기능이 요구되는 응용분야의 경우 한계가 있다.Activated carbon fibers are produced by stabilizing (immobilized) fibers or carbon fibers by activating an oxidizing gas or various salts in a temperature range of 700 to 1200 ° C. to form a myriad of fine pores on the fiber surface. Is a waste of energy in the manufacturing process, there is a restriction in controlling the pore structure. In particular, the chemical activation method using various salts, there is a difficulty in the continuous process and mass production with corrosion of the reactor (carbonization, activation furnace), there is inconvenience to use the acid treatment and neutralization treatment before use. In addition, in the case of activated carbon fibers produced by solution spinning or melt spinning methods, the diameter is in the range of 10-20 μm, so there are limitations in applications requiring a function of requiring fast adsorption and desorption.
본 발명의 목적은 상기한 바와 같은 단점을 갖는 활성화 단계를 거치지 않고 활성탄소 나노섬유 부직포를 제조하는 방법을 제공하는 것이다.It is an object of the present invention to provide a method for producing activated carbon nanofiber nonwovens without undergoing an activation step having the disadvantages described above.
즉, 본 발명은 산화안정화된 나노섬유 부직포를 활성화처리 단계를 거치지 않고 탄소화 처리에 의해 방사시 섬유내부에 함유된 각종 염류가 빠져나오면서 섬유 표면에 무수한 미세공을 형성시켜 체적대비 비표면적이 크고, 세공구조를 조절할 수 있는 활성탄소나노섬유 부직포 제조 방법을 제공하고자 한다.That is, the present invention forms a myriad of fine pores on the surface of the fiber while spinning the carbon nanofibers without spinning the oxidation-stabilized nanofiber nonwoven fabric by the carbonization treatment to form a myriad of fine pores on the surface of the fiber has a large specific surface area To provide a method of manufacturing an activated carbon nanofiber nonwoven fabric that can control the pore structure.
또한, 본 발명은 각종 촉매 담지재, 각종 전극재료(슈퍼캐퍼시터, 연료전지), 고성능 흡착재료 등으로 응용이 가능한 탄소 나노 섬유를 제공하고자 한다.In addition, the present invention is to provide carbon nanofibers that can be applied to various catalyst supporting materials, various electrode materials (supercapacitors, fuel cells), high performance adsorption materials and the like.
도 1은 전기방사 방식을 이용한 활성탄소섬유제조 공정도.1 is an activated carbon fiber manufacturing process using an electrospinning method.
도 2는 PAN에 ZnCl2를 5중량% 함유하여 복합방사한 섬유의 전자현미경 사진.Figure 2 is an electron microscope photograph of a composite spun fibers to contain 5% by weight of ZnCl 2 in the PAN.
도 3은 PAN에 ZnCl2를 0 - 5 중량% 함유하여 복합방사한 섬유의 열중량 분석(thermogravimetric analysis)를 나타낸 그래프.Figure 3 is a graph showing the thermogravimetric analysis of the composite spun fiber containing 0-5% by weight of ZnCl 2 in PAN.
도 4는 ZnCl25중량%를 함유한 나노복합섬유를 800℃ 에서 탄소화한 나노섬유의 전자현미경 사진.Figure 4 is an electron micrograph of the nanofibers carbonized nanocomposite fiber containing 5% by weight of ZnCl 2 at 800 ℃.
도 5는 800 ℃에서 탄소화하여 77K에서 질소 등온흡착을 나타낸 그래프.5 is a graph showing nitrogen isothermal adsorption at 77 K by carbonization at 800 ℃.
도 6는 DFT(Density Functional Theory, 밀도 함수 이론)분석에 의한 세공구조 변화를 나타낸 그래프.Figure 6 is a graph showing the pore structure change by Density Functional Theory (DFT) analysis.
이하 본 발명의 구성을 상세히 설명하면 다음과 같다.Hereinafter, the configuration of the present invention in detail.
본 발명은, 탄소섬유전구체 재료, 무기화합물 및 용매를 혼합하여 방사용액을 제조하는 단계; 상기 제조한 방사용액을 전기방사하여 무기염류가 복합화된 나노섬유를 얻는 단계; 상기 제조한 복합 나노섬유를 공기중에서 0.5 ~ 5℃/min의 승온속도로 250 ~ 350℃까지 승온한 후, 상기 최종온도에서 0.1 ~ 3시간 유지하여 산화 안정화시키는 단계; 상기 산화안정화된 섬유를 불활성 분위기 또는 진공상태에서 500 ~ 1500℃의 온도범위에서 탄소화시키는 단계를 포함하는 것을 특징으로 하는 활성탄소 나노섬유의 제조방법을 제공한다.The present invention comprises the steps of preparing a spinning solution by mixing a carbon fiber precursor material, an inorganic compound and a solvent; Electrospinning the prepared spinning solution to obtain nanofibers having an inorganic salt complexed thereto; Heating the prepared composite nanofibers to 250 to 350 ° C. at a heating rate of 0.5 to 5 ° C./min in air, and then oxidizing and stabilizing the mixture at 0.1 to 3 hours at the final temperature; It provides a method for producing activated carbon nanofibers, comprising the step of carbonizing the oxidative stabilized fibers in a temperature range of 500 ~ 1500 ℃ in an inert atmosphere or vacuum.
또한, 본 발명은 상기 탄소섬유전구체 재료가 폴리아크릴로나이트릴, 셀룰로오스, 피치 및 페놀수지 등으로 구성되는 그룹으로부터 선택되는 1종 이상인 것을 특징으로 하는 활성탄소나노섬유의 제조방법을 제공한다.The present invention also provides a method for producing activated carbon nanofibers, characterized in that the carbon fiber precursor material is at least one member selected from the group consisting of polyacrylonitrile, cellulose, pitch and phenol resin.
또한, 본 발명은, 상기 무기화합물은 ZnCl2, KOH 및 H3PO4으로 이루어지는 그룹으로부터 선택되는 1종 이상인 것을 특징으로 하는 활성탄소나노섬유의 제조방법을 제공한다.The present invention also provides a method for producing activated carbon nanofibers, characterized in that the inorganic compound is at least one member selected from the group consisting of ZnCl 2 , KOH and H 3 PO 4 .
또한, 본 발명은 상기 탄소섬유전구체 재료를 용해할 수 있는 용매가 N,N-디메틸포름 아미드(DMF), 디메틸아세트 아미드(DMAc), 테트라하이드로 퓨란(THF), 질산, 황산, DMSO, Dioxanone 으로부터 선택되는 1종 이상인 것을 특징으로 하는 활성탄소나노섬유 제조방법을 제공한다.In addition, the present invention is a solvent capable of dissolving the carbon fiber precursor material is N, N- dimethylformamide (DMF), dimethylacetamide (DMAc), tetrahydrofuran (THF), nitric acid, sulfuric acid, DMSO, Dioxanone It provides an activated carbon nanofiber manufacturing method characterized in that at least one selected.
또한, 본 발명은, 상기 활성탄소섬유의 직경이 50 - 500 nm 이고, 비표면적이 500 - 3500 ㎡/g인 것을 특징으로 하는 활성탄소나노섬유의 제조방법을 제공한다.The present invention also provides a method for producing activated carbon nanofibers, wherein the activated carbon fibers have a diameter of 50 to 500 nm and a specific surface area of 500 to 3500 m 2 / g.
이하, 첨부된 도면을 통하여 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
먼저, 섬유성형성 고분자와 무기염류를 탄소섬유 전구체 고분자를 용해할 수 있는 용매에 용해하여 방사용액을 제조한다. 상기 섬유성형성 고분자로는 탄소섬유전구체 고분자인 폴리아크릴로나이트릴, 셀룰로오스, 페놀, 피치로 이루어지는 그룹으로부터 선택된 1종 이상을 사용할 수 있으며, 무기화합물로는 ZnCl2, KOH, H3PO4으로부터 이루어지는 그룹으로부터 선택된 1종 이상을 사용할 수 있다. 상기 탄소섬유 전구체 고분자를 용해할 수 있는 방사용매로는, N,N-디메칠포름아미드(DMF), 디메칠아세트 아미드(DMAc), 테트라하이드로 퓨란(THF), 질산, 황산, DMSO, Dioxanone 등의 유기용매 및 산등을 사용할 수 있다.First, a spinning solution is prepared by dissolving a fibrous forming polymer and an inorganic salt in a solvent capable of dissolving a carbon fiber precursor polymer. As the fibrous forming polymer, one or more selected from the group consisting of polyacrylonitrile, cellulose, phenol, and pitch, which are carbon fiber precursor polymers, may be used. As the inorganic compound, ZnCl 2 , KOH, and H 3 PO 4 may be used. One or more types selected from the group consisting of can be used. Examples of the spinning solvent that can dissolve the carbon fiber precursor polymer include N, N-dimethylformamide (DMF), dimethylacetamide (DMAc), tetrahydrofuran (THF), nitric acid, sulfuric acid, DMSO, Dioxanone, and the like. Organic solvents and acids can be used.
다음으로 상기 방사용액을 고전압하에서 전기방사하여 탄소섬유전구체 고분자와 무기염류가 혼합된 형태의 복합섬유를 제조한다. 이때 전기방사는 통상의 전기방사장치를 사용하여 상온, 진공, 온도조절 등의 환경에서 방사를 실시한다.Next, the spinning solution is electrospun under high voltage to produce a composite fiber in which a carbon fiber precursor polymer and an inorganic salt are mixed. At this time, the electrospinning is carried out in an environment such as room temperature, vacuum, temperature control using a conventional electrospinning device.
상기 제조된 복합섬유를 온도조절기와 공기유량을 조절할 수 있는 전기로에 넣고 상온에서 최종온도가 250 ~ 350℃가 되도록 0.5 - 5℃/min 의 승온속도로 승온하여 산화안정화 처리를 하여 불융화 섬유를 얻는다. 이때 ZnCl2등의 염류는 탈수반응을 촉진시켜 불융화 처리를 보다 신속하게 하는 효과가 있으며, 부분적으로 섬유로부터 탈리되기도 한다.Put the prepared fiber into an electric furnace that can control the temperature controller and air flow rate and the temperature is raised at a temperature increase rate of 0.5-5 ℃ / min so that the final temperature is 250 ~ 350 ℃ at room temperature to give an oxidation stabilized treatment Get At this time, salts such as ZnCl 2 have an effect of accelerating the dehydration reaction to speed up the incompatibility treatment, and may be partially detached from the fiber.
제조된 불융화 섬유는 불활성 분위기나 진공상태에서 500 - 1500℃의 온도범위에서 탄소화 처리하여 활성탄소섬유를 얻는다. 이와 같이 얻어진 섬유의 직경은 대략 50 - 500 nm 범위이고, 비표면적은 500 - 3500 ㎡/g 이다.The prepared infusible fibers are carbonized at an inert atmosphere or in a vacuum at a temperature in the range of 500-1500 ° C. to obtain activated carbon fibers. The diameter of the fibers thus obtained is in the range of approximately 50-500 nm and the specific surface area is 500-3500 m 2 / g.
이와 같이, 본 발명의 전구체 방사용액의 처리에 의해 탄소화 과정만으로 체적당 비표면적이 큰 활성탄소섬유의 제조는 각종 산업체에서 촉매담체재료, 전기이중층 슈퍼캐퍼시터용 전극재료, 연료전지 전극재료, 각종 고성능 흡착재료 등으로 다양하게 응용이 가능하다. 또한 본 발명에 의해 제조된 활성탄소섬유를 분쇄하여 사용할 수도 있다.As described above, the production of activated carbon fibers having a large specific surface area per volume only by the carbonization process by treatment of the precursor spinning solution of the present invention has been widely used in various industries, such as catalyst carrier materials, electrode materials for electric double layer supercapacitors, fuel cell electrode materials, Various applications are possible with high performance adsorption materials. In addition, the activated carbon fibers produced by the present invention may be used by grinding.
이하 실시예를 통하여 본 발명을 더욱 구체적으로 살펴본다. 그러나 본 발명이 하기 실시예에만 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the present invention is not limited only to the following examples.
실시예Example
실시예 1Example 1
10 중량%의 폴리아크릴로나이트릴과, ZnCl21-10 중량%를 N,N-디메틸포름아마이드(DMF) 용매에 첨가하고, 60℃에서 1시간 교반한 후 상온에서 다시 24시간 교반하여 방사용액을 제조하였다. 상기 제조한 방사용액은 20kV, 집전체와 방사구와의 거리 20cm, 상온에서 전기방사하여 폴리아크릴로나이트릴에 염화아연이 복합화된 나노섬유를 얻었다. 5중량%의 ZnCl2을 함유하는 복합나노섬유의 전자현미경 사진은 도 2에 나타내었다. 이때 얻어진 섬유의 평균직경은 250nm 정도였다. 염화아연의 첨가량에 따른 복합나노섬유의 열적거동은 도 3에 나타내었는데, 염화아연의 첨가량이 증가할수록 열적거동이 증가하는 것을 알 수 있다. 상기 얻어진 복합섬유를 2℃/min로 승온하여 300℃에서 1시간 공기중에서 산화안정화 처리하여 불융화 섬유를 얻었다. 이때 평균직경은 거의 변화가 없었으며, 산화안정화 처리에 의해 표면이 갈색 또는 흑색으로 변하는 것을 관찰 할 수 있다.10% by weight of polyacrylonitrile and 1-10% by weight of ZnCl 2 are added to a solvent of N, N-dimethylformamide (DMF), and stirred at 60 ° C for 1 hour, followed by another 24 hours at room temperature. The use solution was prepared. The prepared spinning solution was electrospun at 20 kV, a distance of 20 cm between the current collector and the spinneret, and room temperature to obtain nanofibers in which zinc chloride was mixed with polyacrylonitrile. Electron micrograph of the composite nano-fiber containing 5 wt% of ZnCl 2 are shown in Fig. The average diameter of the fiber obtained at this time was about 250 nm. The thermal behavior of the composite nanofibers according to the amount of zinc chloride added is shown in Figure 3, it can be seen that the thermal behavior increases as the amount of zinc chloride increases. The obtained composite fiber was heated to 2 ° C./min, and subjected to oxidative stabilization in air at 300 ° C. for 1 hour to obtain an incompatible fiber. At this time, the average diameter was almost unchanged, and it can be observed that the surface changed to brown or black by oxidative stabilization treatment.
상기 산화안정화 처리된 불융화 섬유를 질소가스나 아르곤가스 등의 불활성 분위기에서 500 - 1500℃ 범위로 탄소화 처리하여 탄소섬유를 제조하였다. 도 4에는 염화아연이 5중량% 첨가된 섬유를 800℃에서 1시간 탄소화 처리된 섬유의 전자현미경 사진을 나타냈다. 얻어진 탄소섬유의 77K에서 질소 등온 흡착곡선을 도 5에 나타내었는데, 상기 도 5에서 보여지는 바와 같이 염화아연의 양이 증가할수록 질소 흡착량이 상대적으로 증가하는 것을 알 수 있으며, 얻어진 등온곡선으로부터 밀도함수이론(DFT, density functional theory)을 사용하여 세공구조를 평가했다(도6). 도 6으로부터, 얻어진 활성탄소 나노섬유의 경우 대부분 마이크로 세공으로 구성되어 있음을 알 수 있었다. 이와 같이 본 발명에 의하면 활성화 공정을 거치지 않고 탄소화 처리에 의해 간단히 활성탄소섬유를 얻을 수 있었다.The oxidative stabilized insoluble fiber was carbonized in an inert atmosphere such as nitrogen gas or argon gas in the range of 500-1500 ° C. to prepare carbon fiber. Figure 4 shows an electron micrograph of the fiber carbonized fiber treated with zinc chloride 5% by weight at 800 ℃ 1 hour. The nitrogen isothermal adsorption curve at 77 K of the obtained carbon fiber is shown in FIG. 5, and as shown in FIG. 5, the nitrogen adsorption amount is relatively increased as the amount of zinc chloride is increased. The pore structure was evaluated using a density functional theory (DFT) (FIG. 6). 6 shows that the activated carbon nanofibers were mostly composed of micropores. As described above, according to the present invention, the activated carbon fibers could be obtained simply by carbonization without undergoing an activation process.
실시예 2Example 2
20중량%의 폴리아크릴로나이트릴에 대해 ZnCl21- 10 중량%를 N,N-디메틸포름아마이드(DMF)와 디메틸아세트아미드(DMAc)의 50/50 중량부의 용매에 첨가하고, 60℃에서 1시간 교반한 후 다시 상온에서 24시간 교반하여 방사용액을 제조하였다. 제조된 방사용액은 20kV, 집전체와 방사구와의 거리 20cm, 상온에서 전기방사하여 폴리아크릴로나이트릴에 염화아연이 복합화된 나노섬유를 얻고, 실시예 1과 같은 방법에 의해 산화안정화 및 탄소화처리하여 활성탄소섬유를 얻었다. 얻어진 활성탄소섬유의 직경은 250nm, 비표면적은 500 - 3500 ㎡/g의 범위였다.To 20% by weight of polyacrylonitrile, 1-10% by weight of ZnCl 2 is added to 50/50 parts by weight of a solvent of N, N-dimethylformamide (DMF) and dimethylacetamide (DMAc) and at 60 ° C. After stirring for 1 hour and again stirred at room temperature for 24 hours to prepare a spinning solution. The prepared spinning solution was electrospun at 20 kV, a distance of 20 cm between the current collector and the spinneret, and electrospun at room temperature to obtain nanofibers in which zinc chloride was mixed with polyacrylonitrile, and subjected to oxidation stabilization and carbonization by the same method as in Example 1. Treatment gave an activated carbon fiber. The diameter of the obtained activated carbon fiber was 250 nm, and the specific surface area was 500-3500 m <2> / g.
본 발명의 방법은 탄소섬유 전구체와 무기화합물을 혼합하여 방사용액을 제조하고 이를 전기방사 한 후 산화안정화 및 탄소화를 거치는 것으로서, 본 발명에 의하면 활성화 과정을 거치지 않고 활성탄소나노섬유를 용이하게 제조할 수 있는 효과가 있다. 또한, 본 발명의 방법에 의해 제조된 활성탄소나노섬유는 체적대비 비표면적이 커, 각종 전극소재, 촉매담체재료, 고성능 흡착재료 등 폭넓은 산업분야에 매우 유용한 활성탄소섬유를 제공할 수 있다.The method of the present invention is to prepare a spinning solution by mixing a carbon fiber precursor and an inorganic compound, and then subjected to oxidation stabilization and carbonization after electrospinning it, according to the present invention to easily prepare activated carbon nanofibers without going through an activation process It can work. In addition, the activated carbon nanofibers produced by the method of the present invention have a large specific surface area to volume, and can provide very useful activated carbon fibers in a wide range of industries such as various electrode materials, catalyst carrier materials, and high performance adsorption materials.
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